Oil-in-water type sunscreen product and preparation method thereof
By using specific thickening agents and dispersion stabilizers in oil-in-water sunscreen products, the product stability and skin irritation problems are solved, and good sun protection effect and refreshing skin feel is achieved, which is suitable for sensitive skin.
Patent Information
- Application Number
- CN202510406783.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-02
- Publication Date
- 2025-06-27
AI Technical Summary
Existing oil-in-water sunscreen products have problems with stability and skin irritation, especially the poor protection effect on sensitive skin, and the powder is poorly dispersed, which is prone to "whitening" problems.
Improve the sun protection effect and stability of the product while reducing skin irritation by using specific ingredients as thickening and dispersion stabilizers in oil-in-water sunscreen products, including carbomer, acrylate/C10-30 alkanol acrylate crosspolymer, hydroxyethyl acrylate/sodium acryloyldimethyltaurate copolymer, disteardimethylammonium hectorite and polyhydroxystearic acid.
It achieves the best sun protection effect, stability and skin-friendliness of oil-in-water sunscreen products. The product has a refreshing skin feeling and good fit, making it suitable for sensitive skin.
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Figure CN120204099A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of cosmetics, and in particular, to an oil-in-water sunscreen product and a preparation method thereof. Background Art
[0002] Generally, sunscreen products such as sunscreen lotions, sunscreen creams, and primers containing physical sunscreens such as titanium dioxide and zinc oxide commonly found on the market are mostly water-in-oil type. Since water-in-oil sunscreen products contain a relatively high content of oils and emulsifiers, they usually result in a thick and greasy skin feel and thus do not provide a good user experience. To reduce the greasy skin feel of sunscreen products, a relatively high content of alcohol or alcohol substitutes generally needs to be added. However, sunscreen products containing a large amount of alcohol may cause irritation to sensitive skin or skin with damaged barriers or further increase the risk of aggravating barrier damage. Moreover, since the powder usually undergoes natural sedimentation and aggregation, the system is unstable and prone to delamination, and the problem of "whitening" is likely to occur. In addition, water-in-oil sunscreen lotions are difficult to clean, and special makeup removers are required to completely remove them. Ordinary facial cleansers may leave residues, thus increasing the burden on the daily sunscreen needs of people with sensitive skin.
[0003] Oil-in-water sunscreen lotions have a moist and refreshing skin feel and can usually be washed off with ordinary facial cleansers, meeting the daily sunscreen needs of people with sensitive skin. Most of the current oil-in-water sunscreen products on the market are pure chemical sunscreen products. Among them, some crystalline chemical sunscreens require a large amount of oil for solubilization to avoid crystal precipitation, and some water-soluble chemical sunscreens need to be neutralized to an alkaline condition to dissolve well without precipitation, resulting in a certain degree of greasiness and irritation. Although the oil-in-water sunscreen products mainly based on physical sunscreens and combined with a small amount of chemical sunscreens can well improve the problems of greasiness and irritation. However, for oil-in-water sunscreen products containing physical sunscreens, due to the ionic solutes of physical sunscreens being extremely likely to have compatibility problems with thickeners, and there are stability problems such as sedimentation, aggregation of powder particles or coalescence of emulsion particles over time or due to temperature changes, the reasonable combination of thickeners and dispersants and the process details of powder dispersion are very important for the stable dispersion of physical sunscreens.
[0004] Therefore, for people with sensitive skin, how to provide a refreshing oil-in-water sunscreen lotion with good sun protection effect, good stability and low irritation is the main technical problem to be solved urgently at present.
[0005] In view of this, the present invention is specifically proposed. Summary of the Invention
[0006] The purpose of the present invention is to provide an oil-in-water sunscreen product and a preparation method thereof to solve or improve the above technical problems.
[0007] The present invention can be realized as follows:
[0008] In a first aspect, the present invention provides an oil-in-water sunscreen product. By weight, the oil-in-water sunscreen product contains 0.01 part to 1 part of a thickener and 0.01 part to 5 parts of a dispersion stabilizer;
[0009] Among them, the thickener includes carbomer, acrylate / C10-30 alkanol acrylate cross-linked polymer, and hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer; the dispersion stabilizer includes dimethyldistearylammonium lithium montmorillonite and polyhydroxystearic acid.
[0010] In an optional embodiment, the thickener includes 0.1 part to 0.2 part of carbomer, 0.05 part to 0.15 part of acrylate / C10-30 alkanol acrylate cross-linked polymer, and 0.1 part to 0.65 part of hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer.
[0011] In an optional embodiment, the dispersion stabilizer includes 0.1 part to 0.5 part of dimethyldistearylammonium lithium montmorillonite and 0.5 part to 0.8 part of polyhydroxystearic acid.
[0012] In an optional embodiment, the oil-in-water sunscreen product further includes at least one of a chelating agent, a preservative, a humectant, an emulsifier, a sunscreen agent, an emollient, a colorant, and a skin conditioner.
[0013] In an optional embodiment, the oil-in-water sunscreen product includes 0.05 part to 0.15 part of a chelating agent, 0.4 part to 0.6 part of a preservative, 2 parts to 10 parts of a humectant, 0.5 part to 5 parts of an emulsifier, 10 parts to 20 parts of a sunscreen agent, 5 parts to 15 parts of an emollient, 2 parts to 4 parts of a colorant, and 0.2 part to 0.5 part of a skin conditioner.
[0014] In an optional embodiment, the chelating agent includes disodium EDTA;
[0015] And / or, the preservative includes p-hydroxyacetophenone;
[0016] And / or, the humectant includes at least one of glycerin, butanediol, propylene glycol, and 1,2-hexanediol;
[0017] And / or, the emulsifier includes at least one of sodium stearoyl glutamate and C12-C20 alkyl glucoside;
[0018] And / or, the sunscreen agent includes at least one of ethylhexyl methoxycinnamate, ethylhexyl triazone, diethylamino hydroxybenzoyl hexyl benzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and titanium dioxide / triethoxysilane octyl;
[0019] And / or, the emollient includes at least one of diisopropyl sebacate, polydimethylsiloxane, and dibutyl adipate;
[0020] And / or, the colorant includes at least one of CI 77891, CI 77489, CI 77491, CI 77492, CI 77499, and CI 77288;
[0021] And / or, the skin conditioner includes at least one of ergothioneine, polygalax urceolata extract, Thermus thermophilus fermentation product, alfalfa extract, and Hormidium iranicum extract.
[0022] In an optional embodiment, the oil-in-water sunscreen product includes 0.1 part of disodium EDTA, 0.5 part of p-hydroxyacetophenone, 3 parts of glycerol, 0.5 part of 1,2-hexanediol, 0.2 part of sodium stearoyl glutamate, 1 part of C12-C20 alkyl glucoside emulsifier, 3 parts of ethylhexyl methoxycinnamate, 1 part of ethylhexyl triazone, 2 parts of diethylamino hydroxybenzoyl hexyl benzoate, 1 part of bis-ethylhexyloxyphenol methoxyphenyl triazine, 8 parts of titanium dioxide / triethoxysilane octyl, 2 parts of diisopropyl sebacate, 2 parts of polydimethylsiloxane, 3 parts of CI 77891, 5 parts of dibutyl adipate, 0.01 part of ergothioneine, 0.1 part of polygalax urceolata extract, 0.1 part of Thermus thermophilus fermentation product, 0.1 part of alfalfa extract, and 0.1 part of Hormidium iranicum extract.
[0023] In a second aspect, the present invention provides a method for preparing an oil-in-water sunscreen product according to any one of the foregoing embodiments, including the following steps: mixing the respective preparation raw materials of the oil-in-water sunscreen product according to a preset ratio.
[0024] In an optional embodiment, the method for preparing an oil-in-water sunscreen product includes the following steps:
[0025] Mix carbomer, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, disodium EDTA with water, heat and stir to obtain an A1 aqueous phase;
[0026] Mix the A1 aqueous phase with p-hydroxyacetophenone, glycerol, and sodium stearoyl glutamate to obtain an A2 aqueous phase;
[0027] Mix diisopropyl sebacate, polydimethylsiloxane, ethylhexyl methoxycinnamate, ethylhexyl triazone, diethylamino hydroxybenzoyl hexyl benzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and C12-C20 alkyl glucoside, heat and stir to obtain a B oil phase;
[0028] Mix CI 77891, dibutyl adipate, lithium magnesium aluminosilicate, polyhydroxystearic acid, and titanium dioxide / triethoxysilane octyl, and pass through a three-roll mill to obtain a C phase;
[0029] Add the C phase to the B oil phase and homogenize to obtain the first mixed phase;
[0030] Add the first mixed phase to the homogenized A2 aqueous phase and homogenize to obtain the second mixed phase;
[0031] Add ergothioneine, Polygonum bistorta extract, Thermus thermophilus fermentation product, Medicago sativa extract, Phormidium persicinum extract and 1,2 - hexanediol to the second mixed phase after cooling, and stir evenly.
[0032] In an alternative embodiment, the A2 aqueous phase is homogenized under the condition of 75 °C to 85 °C;
[0033] And / or, the temperature of the second mixed phase after cooling is 40 °C to 45 °C.
[0034] The beneficial effects of the present invention include:
[0035] The oil - in - water sunscreen product provided by the present invention uses specific components as thickeners and at the same time uses specific components as dispersion stabilizers, enabling the product to have better sun protection effects, good stability, low skin irritation, a refreshing feel and good conformability. Its preparation method is simple, easy to operate and suitable for industrial production. BRIEF DESCRIPTION OF THE DRAWINGS
[0036] To more clearly illustrate the technical solutions of the embodiments of the present invention, the following will briefly introduce the drawings required for use in the embodiments. It should be understood that the following drawings only show some embodiments of the present invention, and therefore should not be regarded as limiting the scope. For those of ordinary skill in the art, other related drawings can be obtained based on these drawings without creative efforts.
[0037] Figure 1 SEM image of the oil - in - water sunscreen product prepared in Example 3;
[0038] Figure 2 SEM image of the oil - in - water sunscreen product prepared in Comparative Example 4;
[0039] Figure 3 Result diagram after centrifugation of the products of Example 3 and Comparative Example 4 in the stability test. DETAILED DESCRIPTION OF THE EMBODIMENTS
[0040] To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. For those conditions not specified in the embodiments, they are carried out according to conventional conditions or the conditions recommended by the manufacturer. For the reagents or instruments not specified by the manufacturer, they are all conventional products that can be obtained through commercial purchase.
[0041] The following specifically describes the oil-in-water sunscreen product provided by the present invention and its preparation method.
[0042] The present invention provides an oil-in-water sunscreen product, which can be, by way of example but not limitation, sunscreen milk, sunscreen cream, primer, or other sunscreen cosmetics.
[0043] By weight, the oil-in-water sunscreen product contains 0.01 part to 1 part of a thickener and 0.01 part to 5 parts of a dispersion stabilizer.
[0044] Exemplarily, the amount of the thickener contained in the oil-in-water sunscreen product can be 0.01 part, 0.05 part, 0.1 part, 0.2 part, 0.5 part, 0.8 part, 1 part, etc., or other values within the range of 0.01 part to 1 part.
[0045] The amount of the dispersion stabilizer contained in the oil-in-water sunscreen product can be 0.01 part, 0.05 part, 0.1 part, 0.5 part, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, etc., or other values within the range of 0.01 part to 5 parts.
[0046] Among them, the thickener can include carbomer, acrylate / C10-30 alkyl acrylate cross-linked polymer, and hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer; the dispersion stabilizer can include dimethyldistearylammonium lithium montmorillonite and polyhydroxystearic acid.
[0047] In some alternative embodiments, the thickener can include 0.1 part to 0.2 part of carbomer, 0.05 part to 0.15 part of acrylate / C10-30 alkyl acrylate cross-linked polymer, and 0.1 part to 0.65 part of hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer.
[0048] The dosage of carbomer can be 0.1 part, 0.15 part, 0.2 part, etc., or other values within the range of 0.1 part to 0.2 part.
[0049] The dosage of acrylate / C10-30 alkyl acrylate cross-linked polymer can be 0.05 part, 0.1 part, 0.15 part, etc., or other values within the range of 0.05 part to 0.15 part.
[0050] The dosage of hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer can be 0.1 part, 0.15 part, 0.2 part, 0.25 part, 0.3 part, 0.35 part, 0.4 part, 0.45 part, 0.5 part, 0.55 part, 0.6 part, 0.65 part, etc., or other values within the range of 0.1 part to 0.65 part.
[0051] The present invention specifically uses 0.1 to 0.2 parts of carbomer in combination with 0.05 to 0.15 parts of acrylate / C10-30 alkyl acrylate cross-linked polymer and 0.1 to 0.65 parts of hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer as thickeners, which can have advantages such as good powder compatibility, strong water-solubilizing feeling, and non-greasy skin feeling compared with other substances that can thicken. If the dosage of carbomer is less than 0.1 part, it is not conducive to increasing the consistency; if the dosage of carbomer is higher than 0.2 part, it is not conducive to providing a fresh and moist skin feeling. If the dosage of acrylate / C10-30 alkyl acrylate cross-linked polymer is less than 0.05 part, it is not conducive to enhancing the emulsification effect; if the dosage of acrylate / C10-30 alkyl acrylate cross-linked polymer is higher than 0.15 part, it is not conducive to the stability of the emulsification interface and the dispersion of the powder. If the dosage of hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer is less than 0.1 part, it is not conducive to increasing the consistency; if the dosage of hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer is higher than 0.65 part, it is not conducive to providing a fresh and moist skin feeling and has a strong sticky feeling.
[0052] In some alternative embodiments, the dispersion stabilizer may include 0.1 to 0.5 parts of lithium magnesium aluminosilicate di-stearyldimonium and 0.5 to 0.8 parts of polyhydroxystearic acid.
[0053] The dosage of lithium magnesium aluminosilicate di-stearyldimonium can be 0.1 part, 0.15 part, 0.2 part, 0.25 part, 0.3 part, 0.35 part, 0.4 part, 0.45 part or 0.5 part, etc., or other values within the range of 0.1 to 0.5 parts.
[0054] The dosage of polyhydroxystearic acid can be 0.5 part, 0.55 part, 0.6 part, 0.65 part, 0.7 part, 0.75 part or 0.8 part, etc., or other values within the range of 0.5 to 0.8 parts.
[0055] The present invention specifically uses 0.1 to 0.5 parts of lithium magnesium aluminosilicate di-stearyldimonium and 0.5 to 0.8 parts of polyhydroxystearic acid as dispersion stabilizers, which can have advantages such as adsorbing on the surface of the physical sunscreen agent, forming uniform dispersed particles, enhancing the system stability, and reducing the sticky feeling compared with other substances that can disperse and stabilize. If the dosage of lithium magnesium aluminosilicate di-stearyldimonium is less than 0.1 part, it is not conducive to forming a uniform dispersed and stable system; if the dosage of lithium magnesium aluminosilicate di-stearyldimonium is higher than 0.5 part, it is not conducive to providing a fresh and moist skin feeling and the system becomes thicker. If the dosage of polyhydroxystearic acid is less than 0.5 part, it is not conducive to the complete adsorption and dispersion of the powder surface to prevent particle aggregation; if the dosage of polyhydroxystearic acid is higher than 0.8 part, it is not conducive to providing a fresh and moist skin feeling and the skin feeling is thick and greasy.
[0056] Furthermore, the oil-in-water sunscreen product provided by the present invention may further include at least one of a chelating agent, a preservative, a humectant, an emulsifier, a sunscreen agent, an emollient, a colorant, and a skin conditioner.
[0057] In some alternative embodiments, the oil-in-water sunscreen product may include 0.05 parts to 0.15 parts (such as 0.05 parts, 0.1 parts, or 0.15 parts, etc.) of a chelating agent, 0.4 parts to 0.6 parts (such as 0.4 parts, 0.45 parts, 0.5 parts, 0.55 parts, or 0.6 parts, etc.) of a preservative, 2 parts to 10 parts (such as 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, or 10 parts, etc.) of a humectant, 0.5 parts to 5 parts (such as 0.5 parts, 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, or 5 parts, etc.) of an emulsifier, 10 parts to 20 parts (such as 10 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, or 20 parts, etc.) of a sunscreen agent, 5 parts to 15 parts (such as 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, or 15 parts, etc.) of an emollient, 2 parts to 4 parts (such as 2 parts, 2.5 parts, 3 parts, 3.5 parts, or 4 parts, etc.) of a colorant, and 0.2 parts to 0.5 parts (such as 0.2 parts, 0.3 parts, 0.4 parts, or 0.5 parts, etc.) of a skin conditioner.
[0058] In some alternative embodiments, the chelating agent may exemplarily but non-exclusively include disodium EDTA.
[0059] The preservative may exemplarily but non-exclusively include p-hydroxyacetophenone.
[0060] The humectant may exemplarily but non-exclusively include at least one of glycerol, butylene glycol, propylene glycol, and 1,2-hexanediol.
[0061] The emulsifier may exemplarily but non-exclusively include at least one of sodium stearoyl glutamate and C12-C20 alkyl glucoside.
[0062] The sunscreen agent may exemplarily but non-exclusively include at least one of ethylhexyl methoxycinnamate, ethylhexyl triazone, diethylamino hydroxybenzoyl hexyl benzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and titanium dioxide / triethoxysilane octyl.
[0063] The emollient may exemplarily but non-exclusively include at least one of diisopropyl sebacate, polydimethylsiloxane, and dibutyl adipate.
[0064] The colorant may include at least one of CI 77891, CI 77489, CI 77491, CI 77492, CI 77499, and CI 77288.
[0065] The skin conditioning agent may illustratively but not limitatively include at least one of ergothioneine, a Cistus polyphyllus extract, a Thermus thermophilus fermentation product, alfalfa extract, and Pseudomonas dasyphylla extract.
[0066] In some optional embodiments, the oil-in-water sunscreen product includes 0.1 parts of disodium EDTA, 0.5 parts of p-hydroxyacetophenone, 3 parts of glycerin, 0.5 parts of 1,2-hexanediol, 0.2 parts of sodium stearoyl glutamate, 1 part of C12-C20 alkyl glucoside emulsifier, 3 parts of ethylhexyl methoxycinnamate, 1 part of ethylhexyl triazone, 2 parts of diethylamino hydroxybenzoyl hexyl benzoate, 1 part of bis-ethylhexyloxyphenol methoxyphenyl triazine, 8 parts of titanium dioxide / triethoxycaprylylsilane, 2 parts of diisopropyl sebacate, 2 parts of polydimethylsiloxane, 3 parts of CI 77891, 5 parts of dibutyl adipate, 0.01 parts of ergothioneine, 0.1 parts of polysaccharide rock rose extract, 0.1 parts of thermophilic Thermus thermophilus fermentation product, 0.1 parts of alfalfa extract and 0.1 parts of Iranian algae extract. The total amount of the above ingredients plus the amount of water is 100 parts.
[0067] Correspondingly, the present invention also provides a method for preparing the above-mentioned oil-in-water type sunscreen product, comprising the following steps: mixing various raw materials for preparing the oil-in-water type sunscreen product according to a preset ratio.
[0068] In some optional embodiments, the method for preparing an oil-in-water sunscreen product comprises the following steps:
[0069] S1: Carbomer, acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, disodium EDTA and water are mixed according to a preset ratio, heated and stirred to obtain an A1 aqueous phase.
[0070] S2: The A1 aqueous phase is mixed with p-hydroxyacetophenone, glycerin and sodium stearoyl glutamate to obtain the A2 aqueous phase.
[0071] S3: Diisopropyl sebacate, dimethicone, ethylhexyl methoxycinnamate, ethylhexyl triazone, diethylamino hydroxybenzoyl hexyl benzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine and C12-C20 alkyl glucoside are mixed, heated and stirred to obtain oil phase B.
[0072] S4: CI 77891, dibutyl adipate, disteardimethylammonium hectorite, polyhydroxystearic acid and titanium dioxide / triethoxyoctylsilane were mixed and passed through a three-roll mill to obtain phase C.
[0073] After the above CI 77891, dibutyl adipate, dimethyldistearylammonium lithium montmorillonite, polyhydroxystearic acid, and titanium dioxide / triethoxyoctylsilane are mixed, aggregates will be formed. In the present invention, the above-mentioned mixed C-phase material is creatively passed through a three-roll mill, and the aggregates can be depolymerized and dispersed by the gaps between adjacent rollers and the strong shearing force and extrusion force between adjacent rollers in the three-roll mill. At the same time, the dispersion stabilizer can better adhere to the surface of the powder, preventing the powder from aggregating again, thereby obtaining fine and uniform materials.
[0074] S5: Add the C phase to the B oil phase and homogenize to obtain the first mixed phase.
[0075] S6: Add the first mixed phase to the homogenized A2 aqueous phase and homogenize to obtain the second mixed phase.
[0076] Exemplarily, the A2 aqueous phase can be homogenized under the condition of 75 °C to 85 °C.
[0077] S7: Add ergothioneine, polytrichum commune extract, thermus thermophilus fermentation product, alfalfa extract, oscillatoria iranica extract, and 1,2-hexanediol to the cooled second mixed phase and stir evenly.
[0078] Exemplarily, the temperature of the cooled second mixed phase can be 40 °C to 45 °C.
[0079] S8: Cool down, defoam, and discharge.
[0080] Continuing from the above, by preparing the oil-in-water sunscreen product with the above raw materials in the above method and order, the resulting product can not only have a better sunscreen effect, but also have a light texture, excellent powder dispersibility, and good conformability.
[0081] The features and properties of the present invention will be further described in detail below in conjunction with examples.
[0082] Example 1
[0083] This example provides an oil-in-water sunscreen primer, and its preparation raw materials are shown in Table 1. The preparation method is as follows:
[0084] S1: According to the ratio in Table 1, mix carbomer, acrylate / C10-30 alkyl acrylate cross-linked polymer, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, disodium EDTA with water, and heat and stir at 80 °C for 10 min to obtain the A1 aqueous phase.
[0085] S2: Mix the A1 aqueous phase with p-hydroxyacetophenone, glycerol, and sodium stearoyl glutamate to obtain the A2 aqueous phase.
[0086] S3: Mix diisopropyl sebacate, polydimethylsiloxane, ethylhexyl methoxycinnamate, ethylhexyl triazone, diethylamino hydroxybenzoyl hexyl benzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and C12-C20 alkyl glucoside, and heat and stir at 85 °C for 5 min to obtain Oil Phase B.
[0087] S4: Mix CI 77891, dibutyl adipate, lithium magnesium silicate di(stearyldimethylammonium), polyhydroxystearic acid, and titanium dioxide / triethoxysilane octyl, and pass through a three-roll mill to obtain Phase C.
[0088] S5: Add Phase C to Oil Phase B and homogenize (80 °C to 85 °C) to obtain the first mixed phase.
[0089] S6: Add the first mixed phase to the homogenized A2 aqueous phase and homogenize (75 °C to 85 °C) to obtain the second mixed phase.
[0090] S7: Add Phase D (ergothioneine, polyumbrella rock rose extract, thermus thermophilus fermentation product, alfalfa extract, oscillatoria iranica extract, and 1,2-hexanediol) to the second mixed phase after cooling (40 °C to 45 °C), and stir evenly.
[0091] S8: Cool to 30 °C, defoam, and discharge.
[0092] The material compositions of the oil-in-water sunscreen lotions provided in Examples 2 to 6 are shown in Table 1, and the preparation methods and conditions are the same as those in Example 1.
[0093] The material compositions of the oil-in-water sunscreen lotions provided in Comparative Examples 1 to 9 are shown in Table 2, and the preparation methods and conditions are the same as those in Example 1.
[0094] The material composition of the oil-in-water sunscreen lotion provided in Comparative Example 10 is basically the same as that in Example 1, except that carbomer is replaced with sodium polyacrylate. The preparation method and conditions are the same as those in Example 1.
[0095] The material composition of the oil-in-water sunscreen lotion provided in Comparative Example 11 is basically the same as that in Example 1, except that acrylate / C10-30 alkyl acrylate crosslinked polymer is replaced with acrylate copolymer. The preparation method and conditions are the same as those in Example 1.
[0096] The material composition of the oil-in-water sunscreen lotion provided in Comparative Example 12 is basically the same as that in Example 1, except that lithium magnesium silicate di(stearyldimethylammonium) is replaced with hectorite. The preparation method and conditions are the same as those in Example 1.
[0097] The material composition of the oil-in-water sunscreen lotion provided in Comparative Example 13 is basically the same as that in Example 1, except that polyhydroxystearic acid is replaced with polyglyceryl-3 diisostearate. The preparation method and conditions are the same as those in Example 1.
[0098] The material composition of the oil-in-water isolation sunscreen lotion provided in Comparative Example 14 is the same as that of Example 1, except that in the preparation process, after mixing CI 77891, dibutyl adipate, dimethyldistearylammonium lithium montmorillonite, polyhydroxystearic acid and titanium dioxide / triethoxyoctylsilane in Step S4, it is not processed by a three-roll mill.
[0099] Table 1 Material Table of Oil-in-Water Isolation Sunscreen Lotion for Examples 1-6
[0100]
[0101]
[0102] Table 2 Material Table of Oil-in-Water Isolation Sunscreen Lotion for Comparative Examples 1-9
[0103]
[0104]
[0105] Test Example
[0106] (1) Product Microstructure Test
[0107] The oil-in-water sunscreen products prepared in Example 3 and Comparative Example 4 were observed by electron microscope, and the results are as Figure 1 and Figure 2 shown.
[0108] Among them, Figure 1 corresponds to the result of Example 3. It can be seen from Figure 1 that the powder in this oil-in-water sunscreen product has excellent dispersibility and no obvious aggregation phenomenon.
[0109] Figure 2 Corresponding to the result of Comparative Example 4, it can be seen from Figure 2 that the powder in this oil-in-water sunscreen product has poor dispersibility and serious powder aggregation.
[0110] (2) Stability Test
[0111] The oil-in-water sunscreen products prepared in Examples 1-6 and Comparative Examples 1-14 were subjected to accelerated stability studies. The specific method was to place the prepared oil-in-water isolation sunscreen lotion at 50°C / 1 month, 40°C / 3 months, 5°C / 3 months, -15°C to 40°C / 6 cycles, and centrifuge: 3000 rpm / 30 min, and observe its layering situation. The results are shown in Table 3 and Figure 3 shown. Figure 3 The left side in the middle corresponds to the result after centrifugation of the product of Example 3, and the right side corresponds to the result after centrifugation of the product of Comparative Example 4.
[0112] Table 3 Test Results
[0113]
[0114]
[0115] From Figure 3 It can be seen that the oil-in-water sunscreen product provided in Example 3 is stable and does not separate into layers after centrifugation, while the oil-in-water sunscreen product provided in Comparative Example 4 separates into layers significantly after centrifugation.
[0116] As can be seen from Table 3:
[0117] Examples 1-4 and Examples 5-6: The compounding of thickeners and dispersants within a certain proportion range can provide stability under extreme conditions. However, in Example 5, slight stratification occurs under centrifugation conditions higher than the national standard (2000 r / min; no stratification for 30 minutes), but the powder dispersion and refreshing skin feel can still meet the expectations; in Example 6, to achieve a higher sun protection effect, a higher proportion of sunscreen agents is added, and the prepared material still has good dispersion and skin feel. However, under extreme cold and heat cycling, the consistency increases and the appearance is slightly rough, but it does not affect the use experience; Example 3 is more refreshing and moisturizing in terms of skin feel.
[0118] Examples 1-4, Comparative Example 1 and Comparative Example 3: When the addition amount of acrylate / C10-30 alkyl acrylate cross-linked polymer is higher than 0.15%, the compatibility with physical sunscreen agents is poor, resulting in powder aggregation and unstable demulsification at the emulsion interface.
[0119] Comparative Examples 5-6: Single dispersants cannot disperse the powder well, and the system is prone to stratification under different temperature conditions.
[0120] Comparative Examples 8-9: The proportion of the dispersant is not within a reasonable range. Although the system can be stable, the skin feel is not refreshing enough, relatively thick and sticky.
[0121] Comparative Examples 10-14: Comparative Example 10 has low thickening efficiency and is prone to stratification; Comparative Examples 11-13 can provide good stability, but the skin feel is sticky; Comparative Example 14 does not perform pre-dispersion treatment on the powder and is prone to coarsening and aggregation.
[0122] (3) Sun Protection Performance Test
[0123] According to the determination method of the sun protection index (SPF value) of sunscreen cosmetics in the "Technical Specifications for Cosmetics Safety" (2015 Edition), the oil-in-water sunscreen products prepared in Examples 1-6 and Comparative Examples 1-14 were tested, and the results are shown in Tables 4 and 5.
[0124] Table 4 Test Results
[0125] Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 SPF 40 38 40 40 20 50
[0126] Table 5 Test Results
[0127]
[0128] It can be seen from Table 4 and Table 5 that:
[0129] Examples 1-4 and Examples 5-6: The compounding of thickeners and dispersion stabilizers within a certain proportion range can provide sunscreen synergistic effect.
[0130] Comparative Examples 1-14: If the thickeners and dispersion stabilizers are not within a reasonable mixing ratio range or the substances of the thickeners and dispersion stabilizers are not properly selected, it will cause the oil-in-water sunscreen products to not exert the sunscreen effect well.
[0131] (4) Safety Test
[0132] Taking the "Technical Specifications for Cosmetics Safety" in 2015 as the reference standard, the oil-in-water sunscreen products prepared in Examples 1-6 were evaluated for cosmetic irritation. The test method was the skin patch test, and 90 people randomly distributed at the age of 21-57 years old were tested (divided into 6 groups).
[0133] Test method: Select qualified patch test equipment. By the closed patch test method, about 0.020 g - 0.025 g (solid or semi-solid) or 0.020 mL - 0.025 mL (liquid) of the test substance was placed in the patch test device, and the external low-sensitivity tape was applied to the back or the flexor side of the forearm of the subject. After 24 hours, the test substance was removed, and the skin reactions were observed at 0.5 h, 24 h, and 48 h after removal, and the results were recorded according to the skin reaction grading standard in the currently effective technical specifications.
[0134] Evaluation criteria:
[0135] Grade 0: Negative reaction;
[0136] Grade 1: Suspected reaction, only faint erythema;
[0137] Grade 2: Weak positive reaction, erythema, infiltration, edema, and papules may occur;
[0138] Grade 3: Strong positive reaction, erythema, infiltration, edema, papules may occur, and the reaction may exceed the test area;
[0139] Grade 4: Extremely strong positive reaction, obvious erythema, severe infiltration, edema, confluent herpes, and the reaction exceeds the test area.
[0140] Test results: The skin reactions of all subjects were negative.
[0141] The above test results show that the oil-in-water sunscreen product provided by the embodiments of the present invention is gentle and non-irritating to the skin and is safe to use. Examples 1 to 6 can all provide an oil-in-water sunscreen primer with a refreshing feel, good conformability, and excellent stability.
[0142] In summary, the oil-in-water sunscreen product provided by the present invention has a better sunscreen effect, good stability, low skin irritation, a refreshing feel, good conformability, and broad application prospects.
[0143] The foregoing is only a preferred embodiment of the present invention and is not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.
Claims
1. An oil-in-water sunscreen product, characterized in that: The oil-in-water sunscreen product contains 0.01 to 1 part of a thickener and 0.01 to 5 parts of a dispersion stabilizer by weight; The thickener includes carbomer, acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer and hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer; the dispersion stabilizer includes disteardimethylammonium hectorite and polyhydroxystearic acid.
2. The oil-in-water sunscreen product according to claim 1, characterized in that: The thickener comprises 0.1 to 0.2 parts of carbomer, 0.05 to 0.15 parts of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer and 0.1 to 0.65 parts of hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer.
3. The oil-in-water sunscreen product according to claim 1, characterized in that: The dispersion stabilizer includes 0.1 to 0.5 parts of disteardimethylammonium hectorite and 0.5 to 0.8 parts of polyhydroxystearic acid.
4. The oil-in-water sunscreen product according to any one of claims 1 to 3, characterized in that: The oil-in-water sunscreen product further comprises at least one of a chelating agent, a preservative, a moisturizer, an emulsifier, a sunscreen, an emollient, a colorant, and a skin conditioner.
5. The oil-in-water sunscreen product according to claim 4, characterized in that: The oil-in-water sunscreen product comprises 0.05 to 0.15 parts of a chelating agent, 0.4 to 0.6 parts of a preservative, 2 to 10 parts of a moisturizing agent, 0.5 to 5 parts of an emulsifier, 10 to 20 parts of a sunscreen, 5 to 15 parts of a moisturizer, 2 to 4 parts of a colorant and 0.2 to 0.5 parts of a skin conditioner.
6. The oil-in-water sunscreen product according to claim 5, characterized in that: The chelating agent includes disodium EDTA; and / or, the preservative comprises p-hydroxyacetophenone; and / or, the humectant comprises at least one of glycerol, butylene glycol, propylene glycol and 1,2-hexanediol; and / or, the emulsifier comprises at least one of sodium stearoyl glutamate and C12-C20 alkyl glucoside; and / or, the sunscreen comprises at least one of ethylhexyl methoxycinnamate, ethylhexyl triazone, diethylamino hydroxybenzoyl hexyl benzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine and titanium dioxide / triethoxycaprylylsilane; and / or, the emollient comprises at least one of diisopropyl sebacate, polydimethylsiloxane and dibutyl adipate; and / or, the colorant comprises at least one of CI 77891, CI 77489, CI 77491, CI 77492, CI 77499 and CI77288; And / or, the skin conditioning agent includes at least one of ergothioneine, a Cistus polyphylla extract, a fermentation product of Thermus thermophilus, alfalfa extract and a Psoralea corylifolia extract.
7. The oil-in-water sunscreen product according to claim 6, characterized in that: The oil-in-water sunscreen product includes 0.1 parts of disodium EDTA, 0.5 parts of p-hydroxyacetophenone, 3 parts of glycerin, 0.5 parts of 1,2-hexanediol, 0.2 parts of sodium stearoyl glutamate, 1 part of C12-C20 alkyl glucoside emulsifier, 3 parts of ethylhexyl methoxycinnamate, 1 part of ethylhexyl triazone, 2 parts of diethylamino hydroxybenzoyl hexyl benzoate, 1 part of bis-ethylhexyloxyphenol methoxyphenyl triazine, 8 parts of titanium dioxide / triethoxycaprylylsilane, 2 parts of diisopropyl sebacate, 2 parts of polydimethylsiloxane, 3 parts of CI 77891, 5 parts of dibutyl adipate, 0.01 parts of ergothioneine, 0.1 parts of polysaccharide rock rose extract, 0.1 parts of thermophilic fermentation product, 0.1 parts of alfalfa extract and 0.1 parts of Iranian algae extract.
8. A method for preparing an oil-in-water sunscreen product according to any one of claims 1 to 7, characterized in that: The method comprises the following steps: mixing various raw materials for preparing oil-in-water type sunscreen products according to a preset ratio.
9. The preparation method according to claim 8, characterized in that: The following steps are involved: Carbomer, acrylic acid (esters) / C10-30 alkyl acrylate cross-linked polymer, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, disodium EDTA and water are mixed according to a preset ratio, heated and stirred to obtain an A1 aqueous phase; Mixing the A1 aqueous phase with p-hydroxyacetophenone, glycerin and sodium stearoyl glutamate to obtain an A2 aqueous phase; Diisopropyl sebacate, polydimethylsiloxane, ethylhexyl methoxycinnamate, ethylhexyl triazone, diethylamino hydroxybenzoyl hexyl benzoate, bis-ethylhexyloxyphenol methoxyphenyl triazine and C12-C20 alkyl glucoside are mixed, heated and stirred to obtain oil phase B; CI 77891, dibutyl adipate, disteardimethylammonium hectorite, polyhydroxystearic acid and titanium dioxide / triethoxyoctylsilane were mixed and passed through a three-roll mill to obtain phase C; Add the phase C to the oil phase B and homogenize to obtain a first mixed phase; Adding the first mixed phase to the homogenized A2 aqueous phase and homogenizing to obtain a second mixed phase; Add ergothioneine, Cistus polyphylla extract, Thermus thermophilus fermentation product, alfalfa extract, Psoralea corylifolia extract and 1,2-hexanediol to the cooled second mixed phase, and stir evenly.
10. The preparation method according to claim 9, characterized in that: The A2 aqueous phase is homogenized at 75°C to 85°C; And / or, the temperature of the second mixed phase after cooling is 40°C to 45°C.
Citation Information
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