A macromolecular sunscreen emulsion and its preparation and application

Abstract

This invention provides a macromolecular sunscreen emulsion, its preparation, and its application. By specifically selecting the types and combinations of dissolving oils and thickeners, and supplementing with other ingredients, this invention yields a macromolecular sunscreen emulsion that not only maintains system stability after being stored in environments with low and high temperatures for three months, exhibiting high stability, but also provides excellent sensory experience and sun protection efficacy. Furthermore, compared to using other dissolving oils and thickeners, the macromolecular sunscreen emulsion of this invention simultaneously possesses superior stability, sensory experience, and sun protection efficacy.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology. More specifically, it relates to a macromolecular sunscreen lotion, its preparation, and its application. Background Technology

[0002] The harmful effects of ultraviolet radiation (UVA and UVB) have been widely confirmed. UVA has strong penetrating power, reaching deep into the dermis, leading to photoaging (such as wrinkles and sagging) and pigmentation (such as age spots); UVB mainly affects the epidermis, causing acute sunburn (such as erythema and edema) and DNA damage (increasing the risk of skin cancer). Sunscreen is currently one of the most commonly used protective measures against the harmful effects of ultraviolet radiation on the skin.

[0003] Macromolecular sunscreens refer to sunscreen ingredients with a molecular weight greater than 500 Da. These sunscreens, especially oil-phase sunscreens (such as diethylhexylbutamidotriazinone, ethylhexyltriazinone, and bis-ethylhexyloxyphenol methoxyphenyltriazine), have a larger molecular weight and are less likely to penetrate the skin, remaining on the skin surface to resist ultraviolet rays, making them relatively safer and more stable. However, these sunscreens are usually more hydrophobic and have more complex molecular structures. When added to sunscreens, they are prone to stability problems such as oiliness, coarsening, or precipitation during long-term storage (3 months) under high and low temperature conditions. Summary of the Invention

[0004] This invention addresses the shortcomings of existing technologies by providing a sunscreen lotion with specific selections of oil-dissolving and thickeners. Even with the addition of oil-phase sunscreen agents with a molecular weight greater than 500 Da, the entire sunscreen lotion system can maintain high stability after being placed in environments such as low and high temperatures for 3 months, while also ensuring excellent sensory experience and sun protection efficacy.

[0005] The above-mentioned objective of this invention is achieved through the following technical solution:

[0006] This invention provides a macromolecular sunscreen emulsion comprising the following components in the following mass percentages: oil-phase sunscreen agent 7.5%–15.5%, aqueous-phase sunscreen agent 3%–6%, oil-soluble powder 8%–15%, emulsifier 2%–5%, emulsion stabilizer 1%–3.5%, thickener 0.4%–1.5%, skin feel modifier 2%–6%, moisturizer 6%–10%, chelating agent 0.02%–0.1%, active ingredient 0.3%–3%, and water to 100%.

[0007] Among them, the molecular weight of oil-phase sunscreen agents is greater than 500 Da;

[0008] The dissolved oils are at least two of the following: butylene glycol dioctanoate / didecanoate, neopentyl glycol diheptanoate, dibutyl adipate, C12-15 benzoate, and diisopropyl sebacate, and the mass percentages of butylene glycol dioctanoate / didecanoate, neopentyl glycol diheptanoate, dibutyl adipate, C12-15 benzoate, and diisopropyl sebacate in the macromolecular sunscreen are 0%–10%, 0–10%, 0–8%, 0–10%, and 0–8%, respectively.

[0009] The thickener is at least one of xanthan gum, sodium polyacrylamide dimethyl taurate, ammonium polyacrylamide dimethyl taurate, and hydroxyethyl cellulose.

[0010] Preferably, the oil-phase sunscreen agent is at least three of the following: diethylhexylbutamidotriazinone, ethylhexyltriazinone, bis-ethylhexyloxyphenol methoxyphenyltriazine, cresoltrazolium trisiloxane, and polysiloxane-15, and the mass percentages of diethylhexylbutamidotriazinone, ethylhexyltriazinone, bis-ethylhexyloxyphenol methoxyphenyltriazine, cresoltrazolium trisiloxane, and polysiloxane-15 in the macromolecular sunscreen emulsion are 1%–3%, 2%–3.5%, 2%–3%, 0%–4%, and 0–2.5%, respectively.

[0011] Preferably, the aqueous sunscreen agent comprises (1) terephthalic methylene dicamphor sulfonic acid or its salts, accounting for 0.5% to 1% by mass in the macromolecular sunscreen emulsion; and (2) methylene bis-benzotriazolyl tetramethyl butylphenol, accounting for 2.5% to 5% by mass in the macromolecular sunscreen emulsion.

[0012] Preferably, the emulsifier is at least two of glyceryl stearate, PEG-100 stearate, cetearyl oleate, sorbitan oleate, arachidonic acid glucoside, and cetyl phosphate potassium, and the mass percentages of glyceryl stearate, PEG-100 stearate, cetearyl oleate, sorbitan oleate, arachidonic acid glucoside, and cetyl phosphate potassium in the macromolecular sunscreen emulsion are 0-2%, 0-2%, 0-2.7%, 0-1.8%, 0-0.5%, and 0.2%-1.5%, respectively.

[0013] Preferably, the emulsifying stabilizer is at least two of cetearyl alcohol, arachidyl alcohol, behenyl alcohol, hydrogenated castor oil, and dextrin palmitate, and the mass percentages of cetearyl alcohol, arachidyl alcohol, behenyl alcohol, hydrogenated castor oil, and dextrin palmitate in the macromolecular sunscreen emulsion are 0-1.5%, 0-1.8%, 0-1%, 0-2%, and 0-0.5%, respectively.

[0014] Preferably, the skin feel modifier is at least two of polydimethylsiloxane, silica, and polymethylsilsesquioxane, and the mass percentages of polydimethylsiloxane, silica, and polymethylsilsesquioxane in the macromolecular sunscreen are 0%–4%, 0%–1%, and 0%–2%, respectively.

[0015] Preferably, the humectant is at least one of dipropylene glycol, 1,3-propanediol, and butylene glycol.

[0016] Preferably, the chelating agent is at least one of disodium EDTA and tetrasodium glutamate diacetate.

[0017] Preferably, the active ingredient is a mixture of water-soluble and oil-soluble active ingredients, and the mass percentages of water-soluble and oil-soluble active ingredients in the macromolecular sunscreen emulsion are 0.2%–2% and 0.1%–1%, respectively.

[0018] More preferably, the water-soluble active ingredient is at least one of Dendrobium officinale extract, Portulaca oleracea extract, allantoin, and dipotassium glycyrrhizate.

[0019] More preferably, the oil-soluble active ingredient is at least one of bisabolol, tocopheryl acetate, and tocopherol (vitamin E).

[0020] As an optional implementation, the macromolecular sunscreen emulsion comprises the following components in the following weight percentages: oil-phase sunscreen agent 7.5%–15.5%, aqueous-phase sunscreen agent 3%–6%, oil-soluble powder 8%–15%, emulsifier 2%–5%, emulsion stabilizer 1%–3.5%, thickener 0.4%–1.5%, skin feel modifier 2%–6%, moisturizer 6%–10%, chelating agent 0.02%–0.1%, active ingredient 0.3%–3%, preservative 0.8%–1.5%, and water to make up to 100%.

[0021] Preferably, the preservative is at least two of phenoxyethanol, ethylhexylglycerin, caprylyl glycol, p-hydroxyacetophenone, and hexanediol, and the mass percentages of phenoxyethanol, ethylhexylglycerin, caprylyl glycol, p-hydroxyacetophenone, and hexanediol in the macromolecular sunscreen are 0%–0.8%, 0%–0.2%, 0–0.2%, 0–0.5%, and 0–1%, respectively.

[0022] As another optional implementation, the macromolecular sunscreen emulsion comprises the following components in the following weight percentages: oil-phase sunscreen agent 7.5%–15.5%, aqueous-phase sunscreen agent 3%–6%, oil-soluble powder 8%–15%, emulsifier 2%–5%, emulsion stabilizer 1%–3.5%, thickener 0.4%–1.5%, skin feel modifier 2%–6%, moisturizer 6%–10%, chelating agent 0.02%–0.1%, active ingredient 0.3%–3%, fragrance 0.05%–0.3%, and water to make up to 100%.

[0023] As another alternative implementation, the macromolecular sunscreen emulsion comprises the following components in the following weight percentages: oil-phase sunscreen agent 7.5%–15.5%, aqueous-phase sunscreen agent 3%–6%, oil-soluble powder 8%–15%, emulsifier 2%–5%, emulsion stabilizer 1%–3.5%, thickener 0.4%–1.5%, skin feel modifier 2%–6%, moisturizer 6%–10%, chelating agent 0.02%–0.1%, active ingredient 0.3%–3%, preservative 0.8%–1.5%, fragrance 0.05%–0.3%, and water to make up to 100%.

[0024] Preferably, the preservative is at least two of phenoxyethanol, ethylhexylglycerin, caprylyl glycol, p-hydroxyacetophenone, and hexanediol, and the mass percentages of phenoxyethanol, ethylhexylglycerin, caprylyl glycol, p-hydroxyacetophenone, and hexanediol in the macromolecular sunscreen are 0%–0.8%, 0%–0.2%, 0–0.2%, 0–0.5%, and 0–1%, respectively.

[0025] Based on this, the present invention also provides a method for preparing the above-mentioned macromolecular sunscreen lotion, comprising the following steps:

[0026] S1. Aqueous phase: Dissolve terephthaloyl dicamphor sulfonic acid or its salts in water, then add thickener, humectant, and chelating agent and mix well;

[0027] S2. Oil phase: Add the oil phase sunscreen to the dissolved oil, heat until dissolved, add emulsifier and emulsion stabilizer and dissolve until transparent, then continue to add oil-soluble active ingredients and skin feel modifier and mix well;

[0028] S3. After adjusting the temperature of the aqueous phase and oil phase to 80-85 ℃, add the oil phase to the aqueous phase and mix well. After homogenization, cool down, then add methylenebis-benzotriazolyltetramethylbutylphenol, water-soluble active ingredient, optional preservative, and optional fragrance. Mix well and degas to obtain the final product.

[0029] Preferably, the mixing described in S1 is achieved by stirring.

[0030] More preferably, the stirring speed is 400-600 rpm.

[0031] Preferably, the heating temperature in S2 is 90–100 °C.

[0032] Preferably, after heating as described in S2, ultrasound is also performed.

[0033] More preferably, the power of the ultrasound is 300-500 W.

[0034] More preferably, the temperature of the ultrasound is 60–80 °C.

[0035] More preferably, the ultrasound duration is 30–60 minutes.

[0036] Preferably, the mixing in S2 is achieved by stirring.

[0037] More preferably, the stirring speed is 500-800 rpm.

[0038] Preferably, the process of adding the oil phase to the water phase and mixing it as described in step S3 is achieved by stirring.

[0039] More preferably, the stirring speed is 500-800 rpm.

[0040] Preferably, the rotational speed of the homogenizer in S3 is 9000 to 12000 rpm.

[0041] Preferably, the homogenization time in S3 is 5 to 10 minutes.

[0042] Preferably, the cooling in S3 is reduced to 45-55°C.

[0043] Preferably, the cooling in S3 is achieved by stirring, such as stirring at 300-400 rpm.

[0044] Preferably, the addition of methylenebis-benzotriazolyltetramethylbutylphenol, water-soluble active ingredient, optional preservative, and optional fragrance in step S3 is achieved by stirring, such as stirring at 300-400 rpm.

[0045] Preferably, the degassing in S3 is achieved by evacuating the system.

[0046] The present invention has the following beneficial effects:

[0047] This invention, through the specific selection and combination of oil-dissolving agents and thickeners, along with other ingredients, yields a macromolecular sunscreen lotion that not only maintains system stability after being stored in environments with low and high temperatures for three months, demonstrating high stability, but also offers excellent sensory experience and sun protection efficacy. Furthermore, compared to using other oil-dissolving agents and thickeners, this invention's macromolecular sunscreen lotion simultaneously possesses superior stability, sensory experience, and sun protection efficacy. Detailed Implementation

[0048] The present invention will be further illustrated below with reference to specific embodiments, but the embodiments do not limit the present invention in any way. Unless otherwise specified, the reagents, methods, and equipment used in the present invention are conventional reagents, methods, and equipment in this technical field.

[0049] Unless otherwise specified, all raw materials used in the following examples and comparative examples are commercially available, and the unit "%" used for raw materials refers to the mass percentage of the raw material in the macromolecular sunscreen emulsion.

[0050] Example 1: A macromolecular sunscreen lotion

[0051] I. Components including the following mass percentages

[0052] Oil-phase sunscreen agents: diethylhexylbutamidotriazinone 2.5%, ethylhexyltriazinone 3%, bis-ethylhexyloxyphenol methoxyphenyl triazine 2.5%, cresoltrazol trisiloxane 2%;

[0053] Aqueous sunscreen agents: 1% terephthalomethyl dicamphor sulfonic acid, 3% methylene bis-benzotriazolyl tetramethylbutylphenol;

[0054] To dissolve oils: 8% dibutyl adipic acid, 1% C12-15 benzoyl alcohol;

[0055] Emulsifiers: 1% glyceryl stearate, 1% PEG-100 stearate, 0.09% arachidonic acid glucoside, 1% potassium cetyl phosphate;

[0056] Emulsifying stabilizers: cetearyl alcohol 1.2%, arachidonic acid 0.33%, behenol 0.18%, dextrin palmitate 0.1%;

[0057] Thickeners: xanthan gum 0.15%, sodium polyacrylamide dimethyl taurate 0.35%;

[0058] Skin feel modifiers: 3% polydimethylsiloxane, 0.5% silica, 1% polymethylsilsesquioxane;

[0059] Moisturizers: Dipropylene glycol 5%, Butylene glycol 2%;

[0060] Chelating agent: 0.05% disodium EDTA;

[0061] Active ingredients: (1) Water-soluble active ingredients: Dendrobium officinale extract 0.1%, Portulaca oleracea extract 1%, allantoin 0.1%; (2) Oil-soluble active ingredients: Bisabolol 0.2%, tocopheryl acetate 0.1%;

[0062] Water: Replenish to 100%.

[0063] II. Preparation Method

[0064] S1. Aqueous phase: Add terephthaloyl dicamphor sulfonic acid to water, then add thickener, humectant, and chelating agent, and stir at 500 rpm until well mixed;

[0065] S2. Oil phase: Add the oil phase sunscreen to the dissolved oil, heat at 95 ℃ until dissolved, then sonicate at 400 W and 70 ℃ for 45 min. Add emulsifier and emulsion stabilizer to dissolve until transparent, then continue to add oil-soluble active ingredients and skin feel modifier and stir at 650 rpm until well mixed.

[0066] S3. After adjusting the temperature of the aqueous phase and oil phase to 85 ℃, add the oil phase to the aqueous phase and mix at 650 rpm. Homogenize at 10000 rpm for 8 min, then cool down to 50 ℃ while stirring at 350 rpm. Add methylenebis-benzotriazolyltetramethylbutylphenol and water-soluble active ingredients and stir at 350 rpm to mix. Degas under vacuum to obtain the final product.

[0067] Example 2: A macromolecular sunscreen lotion

[0068] I. Components including the following mass percentages

[0069] Same as Example 1, except that:

[0070] (1) Replace the dissolved oil with: 10% butanediol dioctanoate / didecanoate and 2% neopentyl glycol diheptanoate;

[0071] (2) Replace the thickener with: 0.8% ammonium polyacrylamide dimethyl taurate and 0.2% hydroxyethyl cellulose.

[0072] II. Preparation Method

[0073] Same as Example 1.

[0074] Example 3: A macromolecular sunscreen lotion

[0075] I. Components including the following mass percentages

[0076] Same as Example 1, except that:

[0077] (1) Replace the dissolved oil with: 8% diisopropyl sebacate and 2% butanediol dioctanoic acid / didecanoate;

[0078] (2) Replace the thickener with xanthan gum 0.4%.

[0079] II. Preparation Method

[0080] Same as Example 1.

[0081] Example 4: A macromolecular sunscreen lotion

[0082] I. Components including the following mass percentages

[0083] Same as Example 1, except that:

[0084] (1) Replace the dissolved oil with: 10% neopentyl glycol diheptate, 2% dibutyl adipate, and 3% C12-15 alcohol benzoate;

[0085] (2) Replace the thickener with: xanthan gum 0.2% and sodium polyacrylamide dimethyl taurate 1.3%.

[0086] II. Preparation Method

[0087] Same as Example 1.

[0088] Example 5: A macromolecular sunscreen lotion

[0089] I. Components including the following mass percentages

[0090] Same as Example 1, except that:

[0091] (1) Replace the dissolved oil with: 2% butanediol dioctanoic acid / didecanoate and 6% dibutyl adipate;

[0092] (2) Replace the thickener with: sodium polyacrylamide dimethyl taurate 0.6% and hydroxyethyl cellulose 0.2%.

[0093] II. Preparation Method

[0094] Same as Example 1.

[0095] Example 6: A macromolecular sunscreen lotion

[0096] I. Components including the following mass percentages

[0097] Same as Example 1, except that:

[0098] (1) Replace the oil phase sunscreen with: 1% diethylhexylbutamidotriazinone, 2.5% ethylhexyltriazinone, 3% bis-ethylhexyloxyphenol methoxyphenyl triazine, and 1.5% polysiloxane-15;

[0099] (2) Replace the aqueous sunscreen agent with: 1% terephthalic methylene dicamphor sulfonic acid and 5% methylene bis-benzotriazolyl tetramethyl butylphenol;

[0100] (3) Replace the dissolved oil with: 5% butanediol dioctanoic acid / didecanoate and 4% diisopropyl sebacate;

[0101] (4) Replace the thickener with: xanthan gum 0.2% and polyacrylamide dimethyl taurate ammonium 0.6%.

[0102] II. Preparation Method

[0103] Same as Example 1.

[0104] Example 7: A macromolecular sunscreen lotion

[0105] I. Components including the following mass percentages

[0106] Same as Example 1, except that:

[0107] (1) Replace the oil phase sunscreen with: 3% diethylhexylbutamidotriazine, 3% ethylhexyltriazine, 3% bis-ethylhexyloxyphenol methoxyphenyl triazine, 4% cresoltrazol trisiloxane, and 2.5% polysiloxane-15;

[0108] (2) Replace the aqueous sunscreen with: 0.5% terephthalic dicamphor sulfonate and 2.5% methylene bis-benzotriazolyl tetramethyl butylphenol;

[0109] (3) Replace the dissolved oil with: 10% C12-15 alcohol benzoate and 5% dibutyl adipic acid;

[0110] (4) Replace the thickener with: xanthan gum 0.3% and sodium polyacrylamide dimethyl taurate 1.2%.

[0111] II. Preparation Method

[0112] S1. Aqueous phase: Dissolve terephthalimide dicamphor sulfonate in water, then add thickener, humectant, and chelating agent, and stir at 500 rpm until well mixed;

[0113] S2. Oil phase: Add the oil phase sunscreen to the dissolved oil, heat at 95 ℃ until dissolved, then sonicate at 400 W and 70 ℃ for 45 min. Add emulsifier and emulsion stabilizer to dissolve until transparent, then continue to add oil-soluble active ingredients and skin feel modifier and stir at 650 rpm until well mixed.

[0114] S3. After adjusting the temperature of the aqueous phase and oil phase to 85 ℃, add the oil phase to the aqueous phase and mix at 650 rpm. Homogenize at 10000 rpm for 8 min, then cool down to 50 ℃ while stirring at 350 rpm. Add methylenebis-benzotriazolyltetramethylbutylphenol and water-soluble active ingredients and stir at 350 rpm to mix. Degas under vacuum to obtain the final product.

[0115] Example 8: A macromolecular sunscreen lotion

[0116] I. Components including the following mass percentages

[0117] Same as Example 1, except that:

[0118] (1) Replace the oil phase sunscreen with: 2% diethylhexylbutamidotriazine, 2% ethylhexyltriazine, 2% bis-ethylhexyloxyphenol methoxyphenyltriazine, 1% cresoltrazol trisiloxane, and 2% polysiloxane-15;

[0119] (2) Replace the aqueous sunscreen agent with: 1% terephthalic methylene dicamphor sulfonic acid and 5% methylene bis-benzotriazolyl tetramethyl butylphenol;

[0120] (3) Replace the dissolved oil with: 4% butanediol dioctanoic acid / didecanoate and 4% C12-15 alcohol benzoate;

[0121] (4) Replace the thickener with: sodium polyacrylamide dimethyl taurate 0.7%.

[0122] II. Preparation Method

[0123] Same as Example 1.

[0124] Example 9: A macromolecular sunscreen lotion

[0125] I. Components including the following mass percentages

[0126] Same as Example 1, except that:

[0127] (1) Replace the oil phase sunscreen with: 1.5% diethylhexylbutamidotriazinone, 3.5% ethylhexyltriazinone, and 2.5% bis-ethylhexyloxyphenol methoxyphenyltriazine;

[0128] (2) Replace the aqueous sunscreen with: 0.8% terephthalic dicamphor sulfonate and 4.3% methylene bis-benzotriazolyl tetramethyl butylphenol;

[0129] (3) Replace the dissolved oil with: 4% C12-15 alcohol benzoate, 4% dibutyl adipate, and 4% diisopropyl sebacate;

[0130] (4) Replace the thickener with: 1% ammonium polyacrylamide dimethyl taurate and 0.2% hydroxyethyl cellulose.

[0131] II. Preparation Method

[0132] S1. Aqueous phase: Dissolve terephthalimide dicamphor sulfonate in water, then add thickener, humectant, and chelating agent, and stir at 500 rpm until well mixed;

[0133] S2. Oil phase: Add the oil phase sunscreen to the dissolved oil, heat at 95 ℃ until dissolved, then sonicate at 400 W and 70 ℃ for 45 min. Add emulsifier and emulsion stabilizer to dissolve until transparent, then continue to add oil-soluble active ingredients and skin feel modifier and stir at 650 rpm until well mixed.

[0134] S3. After adjusting the temperature of the aqueous phase and oil phase to 85 ℃, add the oil phase to the aqueous phase and mix at 650 rpm. Homogenize at 10000 rpm for 8 min, then cool down to 50 ℃ while stirring at 350 rpm. Add methylenebis-benzotriazolyltetramethylbutylphenol and water-soluble active ingredients and stir at 350 rpm to mix. Degas under vacuum to obtain the final product.

[0135] Example 10: A macromolecular sunscreen lotion

[0136] I. Components including the following mass percentages

[0137] Same as Example 1, except that:

[0138] (1) Replace the emulsifier with: 2.7% cetearyl oleate, 1.8% sorbitan oleate, and 0.5% cetearyl phosphate potassium;

[0139] (2) Replace the emulsifying stabilizer with: behenol 0.5% and dextrin palmitate 0.5%;

[0140] (3) Replace the skin feel modifier with: 1% silica and 1% polymethylsilsesquioxane;

[0141] (4) Replace the moisturizer with: 5% 1,3-propanediol and 5% butylene glycol;

[0142] (5) Replace the chelating agent with: 0.05% tetrasodium glutamate diacetate;

[0143] (6) Replace the active ingredients with: (1) water-soluble active ingredient: Dendrobium officinale extract 0.2%; (2) oil-soluble active ingredient: bisabolol 0.1%;

[0144] (7) The preservatives added are: phenoxyethanol 0.8%, ethylhexylglycerin 0.2%, and octyl glycol 0.2%;

[0145] (8) Add 0.2% of fragrance.

[0146] II. Preparation Method

[0147] S1. Aqueous phase: Add terephthaloyl dicamphor sulfonic acid to water, then add thickener, humectant, and chelating agent, and stir at 500 rpm until well mixed;

[0148] S2. Oil phase: Add the oil phase sunscreen to the dissolved oil, heat at 95 ℃ until dissolved, then sonicate at 400 W and 70 ℃ for 45 min. Add emulsifier and emulsion stabilizer to dissolve until transparent, then continue to add oil-soluble active ingredients and skin feel modifier and stir at 650 rpm until well mixed.

[0149] S3. After adjusting the temperature of the aqueous phase and oil phase to 85 ℃, add the oil phase to the aqueous phase and mix at 650 rpm. Homogenize at 10000 rpm for 8 min, then cool to 50 ℃ while stirring at 350 rpm. Add methylenebis-benzotriazolyltetramethylbutylphenol, water-soluble active ingredients, preservatives, and fragrances, and stir and mix at 350 rpm. Degas under vacuum to obtain the final product.

[0150] Example 11 A macromolecular sunscreen lotion

[0151] I. Components including the following mass percentages

[0152] Same as Example 1, except that:

[0153] (1) Replace the emulsifier with: 0.5% arachidonic acid glucoside and 1.5% potassium cetyl phosphate;

[0154] (2) Replace the emulsifying stabilizer with: 0.2% cetearyl alcohol, 1.8% arachidonic acid, and 1% behenol;

[0155] (3) Replace the skin feel modifier with: 2% polydimethylsiloxane and 0.5% silica;

[0156] (4) Replace the moisturizer with: 6% dipropylene glycol;

[0157] (5) Replace the chelating agent with: 0.02% tetrasodium glutamate diacetate;

[0158] (6) Replace the active ingredients with: (1) Water-soluble active ingredients: purslane extract 1.75%, dipotassium glycyrrhizate 0.05%, allantoin 0.2%; (2) Oil-soluble active ingredients: bisabolol 0.3%, tocopherol (vitamin E) 0.7%;

[0159] (7) The preservatives added are: phenoxyethanol 0.5%, ethylhexylglycerin 0.1%, and p-hydroxyacetophenone 0.2%;

[0160] (8) Add 0.05% of fragrance.

[0161] II. Preparation Method

[0162] S1. Aqueous phase: Add terephthaloyl dicamphor sulfonic acid to water, then add thickener, humectant, and chelating agent, and stir at 600 rpm until well mixed;

[0163] S2. Oil phase: Add the oil phase sunscreen to the dissolved oil, heat at 90 ℃ until dissolved, then sonicate at 500 W and 60 ℃ for 60 min. Add emulsifier and emulsion stabilizer to dissolve until transparent, then continue to add oil-soluble active ingredients and skin feel modifier and stir at 500 rpm to mix well.

[0164] S3. After adjusting the temperature of the aqueous phase and oil phase to 80 ℃, add the oil phase to the aqueous phase and mix at 500 rpm. Homogenize at 12000 rpm for 5 min, then cool down to 45 ℃ while stirring at 400 rpm. Add methylenebis-benzotriazolyltetramethylbutylphenol, water-soluble active ingredients, preservatives, and fragrances, and stir and mix at 400 rpm. Degas under vacuum to obtain the final product.

[0165] Example 12 A macromolecular sunscreen lotion

[0166] I. Components including the following mass percentages

[0167] Same as Example 1, except that:

[0168] (1) Replace the emulsifier with: 2% glyceryl stearate, 2% PEG-100 stearate, and 0.2% potassium cetyl phosphate;

[0169] (2) Replace the emulsifying stabilizer with: 1.5% cetearyl alcohol and 2% hydrogenated castor oil;

[0170] (3) Replace the skin feel modifier with: 4% polydimethylsiloxane and 2% polymethylsilsesquioxane;

[0171] (4) Replace the moisturizer with: 2% 1,3-propanediol and 4% dipropylene glycol;

[0172] (5) Replace the chelating agent with: 0.1% tetrasodium glutamate diacetate;

[0173] (6) Replace the active ingredients with: (1) water-soluble active ingredients: purslane extract 1%, allantoin 0.2%; (2) oil-soluble active ingredients: bisabolol 0.3%, tocopheryl acetate 0.5%;

[0174] (7) The preservatives are: 0.5% p-hydroxyacetophenone and 1% hexanediol;

[0175] (8) Add 0.3% of flavoring.

[0176] II. Preparation Method

[0177] S1. Aqueous phase: Add terephthaloyl dicamphor sulfonic acid to water, then add thickener, humectant, and chelating agent, and stir at 400 rpm until well mixed;

[0178] S2. Oil phase: Add the oil phase sunscreen to the dissolved oil, heat at 100 ℃ until dissolved, then sonicate at 300 W and 80 ℃ for 30 min. Add emulsifier and emulsion stabilizer to dissolve until transparent, then continue to add oil-soluble active ingredients and skin feel modifier and stir at 800 rpm until well mixed.

[0179] S3. After adjusting the temperature of the aqueous phase and oil phase to 85 ℃, add the oil phase to the aqueous phase and mix at 800 rpm. Homogenize at 9000 rpm for 10 min, then cool down to 55 ℃ while stirring at 300 rpm. Add methylenebis-benzotriazolyltetramethylbutylphenol, water-soluble active ingredients, preservatives, and fragrances, and stir and mix at 300 rpm. Degas under vacuum to obtain the final product.

[0180] Example 13 A macromolecular sunscreen lotion

[0181] I. Components including the following mass percentages

[0182] Same as Example 1.

[0183] II. Preparation Method

[0184] Same as Example 1, except that S2 does not involve ultrasound, that is, S2 is as follows:

[0185] S2. Oil phase: Add the oil phase sunscreen to the dissolved oil, heat at 95 ℃ until dissolved, add emulsifier and emulsion stabilizer and dissolve until transparent, then continue to add oil-soluble active ingredients and skin feel modifier and stir at 650 rpm until well mixed.

[0186] Comparative Example 1

[0187] Same as Example 1, except that dibutyl adipic acid is replaced with an equal mass of triglyceride (ethylhexanoate) in the oil.

[0188] Comparative Example 2

[0189] Same as Example 1, except that the C12-15 alcohol benzoate in the dissolved oil is replaced with an equal mass of neopentyl glycol di(ethylhexanoate).

[0190] Comparative Example 3

[0191] Same as Example 1, except that dibutyl adipic acid is replaced with an equal mass of isononyl isononanoate in the oil.

[0192] Comparative Example 4

[0193] Same as Example 1, except that dibutyl adipic acid is replaced with an equal mass of cetyl ethylhexanoate in the oil.

[0194] Comparative Example 5

[0195] Same as Example 1, except that the dissolved oil is replaced with: 8% hydrogenated polyisobutylene and 1% lauryl lactate.

[0196] Comparative Example 6

[0197] Same as Example 2, except that butanediol dioctanoate / didecanoate in the dissolved oil is replaced with an equal mass of ethylhexyl palmitate.

[0198] Comparative Example 7

[0199] Same as Example 3, except that the diisopropyl sebacate dissolved in the oil is replaced with an equal mass of caprylic / capric triglyceride.

[0200] Comparative Example 8

[0201] Same as Example 1, except that xanthan gum in the thickener is replaced with an equal mass of gellan gum.

[0202] Comparative Example 9

[0203] Same as Example 1, except that sodium polyacrylamide dimethyl taurate in the thickener is replaced with an equal mass of ammonium acrylamide dimethyl taurate / VP copolymer.

[0204] Test Example 1: Stability Test

[0205] The macromolecular sunscreens obtained in Examples 1-13 and Comparative Examples 1-9 were placed in environments of -18, 4, 25, and 45 °C for 3 months, respectively, and the results were observed to see whether unstable phenomena such as oiling, coarsening, and precipitation occurred. The results are shown in Table 1.

[0206] Table 1

[0207]

[0208] In the table, "OK" indicates that the material is a uniform and continuous emulsion without any unstable phenomena such as oiling, coarsening, or precipitation; "precipitation" indicates that white solid particles are precipitated from the material; "coarsening" indicates that the material has a rough, clumpy feel; "slight oiling" indicates that a small amount of oil is precipitated on the surface of the material and accumulates on the bottle wall; "oiling" indicates that a large amount of oil is precipitated on the surface of the material, and a layer of transparent oil can be clearly seen floating on the surface of the material.

[0209] It is evident that the macromolecular sunscreens obtained in Examples 1-13 exhibit better stability, while the macromolecular sunscreens obtained in Comparative Examples 1-9 all show some degree of instability. This indicates that it is precisely through the specific selection and combination of dissolving oils and thickeners, along with other ingredients, that the macromolecular sunscreens obtained in this invention can maintain system stability after being placed in environments such as low temperature and high temperature for 3 months, demonstrating high stability.

[0210] Test Example 2: Security Test

[0211] According to the human skin patch test method in the 2015 edition of the "Cosmetic Safety Technical Specifications", patch tests were conducted on 30 people with the macromolecular sunscreens obtained in Examples 1 to 13. All test results were negative, indicating that the macromolecular sunscreens of the present invention have high safety.

[0212] Test Example 3: Sensory Evaluation

[0213] Ten evaluators (aged 20-35) who had undergone three months of standardized sensory evaluation training were selected to conduct sensory tests on the macromolecular sunscreens obtained in Examples 1-13 and Comparative Examples 1-9. The testing environment was maintained at a constant temperature and humidity (temperature 20-22 ℃, relative humidity 50%-60%). The same area on the inside of the evaluator's left arm was designated as the test area. After each test of a macromolecular sunscreen, the test area was required to be thoroughly cleaned, and the evaluator was required to sit quietly in the testing environment for 30 minutes before conducting the sensory evaluation of the next macromolecular sunscreen.

[0214] Take a soybean-sized amount of the macromolecular sunscreen obtained in Examples 1-13 and Comparative Examples 1-9, and apply it to the test area at a speed of 1 second per circle. After spreading evenly (if it is not spread evenly after more than 10 circles, 10 circles are taken as the end point), score the spreadability, greasiness, and stickiness of the macromolecular sunscreen according to the standard of 0-10. The result is the average score of 10 evaluators. Finally, the average scores of the three sensory indicators of spreadability, greasiness, and stickiness are added together to obtain the total sensory score. The results are shown in Table 2. Among them, spreadability evaluates the ease of applying macromolecular sunscreen, 0 points (difficult) → 10 points (easy); greasiness evaluates the oiliness of the skin after application, 0 points (strong) → 10 points (weak); stickiness evaluates the adhesion between the skin and fingers after application, 0 points (strong) → 10 points (weak).

[0215] Table 2

[0216]

[0217] It is evident that the overall sensory scores of the macromolecular sunscreens obtained in Examples 1-13 are significantly better than those in Comparative Examples 1-9. This indicates that it is precisely because of the specific selection of the types and combinations of oil-dissolving agents and thickeners, along with other ingredients, that the macromolecular sunscreens obtained in this invention can have such an excellent sensory experience. They are not only easy to apply, but also do not produce an oily or sticky feeling on the skin after application.

[0218] Test Example 4: Sunscreen Performance Test

[0219] According to the determination methods for the sun protection factor (SPF) and long-wave ultraviolet protection factor (PFA) of sunscreen cosmetics in the "Cosmetic Safety Technical Specifications" (2015 edition), the sun protection performance of the macromolecular sunscreen lotions obtained in Examples 1-2, 7-8, 10, and 12 was tested, and the results are shown in Table 3.

[0220] Table 3

[0221]

[0222] As can be seen, the SPF values ​​of the macromolecular sunscreens obtained in Examples 1-2, 7-8, 10, and 12 are all above 50, and the PFA values ​​are all above 10, indicating that the macromolecular sunscreens of the present invention have strong UV protection performance and excellent sun protection efficacy.

[0223] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A macromolecular sunscreen lotion, characterized in that, The product comprises the following components by weight percentage: oil-phase sunscreen 7.5%–15.5%, aqueous-phase sunscreen 3%–6%, oil-soluble powder 8%–15%, emulsifier 2%–5%, emulsion stabilizer 1%–3.5%, thickener 0.4%–1.5%, skin feel modifier 2%–6%, moisturizer 6%–10%, chelating agent 0.02%–0.1%, active ingredient 0.3%–3%, and water to 100%. Among them, the molecular weight of oil-phase sunscreen agents is greater than 500 Da; The dissolved oils are at least two of the following: butylene glycol dioctanoate / didecanoate, neopentyl glycol diheptanoate, dibutyl adipate, C12-15 benzoate, and diisopropyl sebacate, and the mass percentages of butylene glycol dioctanoate / didecanoate, neopentyl glycol diheptanoate, dibutyl adipate, C12-15 benzoate, and diisopropyl sebacate in the macromolecular sunscreen are 0%–10%, 0–10%, 0–8%, 0–10%, and 0–8%, respectively. The thickener is at least one of xanthan gum, sodium polyacrylamide dimethyl taurate, ammonium polyacrylamide dimethyl taurate, and hydroxyethyl cellulose; The oil-phase sunscreen agent is at least three of the following: diethylhexylbutamidotriazinone, ethylhexyltriazinone, bis-ethylhexyloxyphenol methoxyphenyltriazine, cresoltrazolium trisiloxane, and polysiloxane-15, and the mass percentages of diethylhexylbutamidotriazinone, ethylhexyltriazinone, bis-ethylhexyloxyphenol methoxyphenyltriazine, cresoltrazolium trisiloxane, and polysiloxane-15 in the macromolecular sunscreen emulsion are 1%–3%, 2%–3.5%, 2%–3%, 0%–4%, and 0–2.5%, respectively. The aqueous sunscreen contains (1) terephthalic dimethylene camphor sulfonic acid or its salts, which account for 0.5% to 1% of the mass of the macromolecular sunscreen emulsion; and (2) methylene bis-benzotriazolyl tetramethyl butylphenol, which account for 2.5% to 5% of the mass of the macromolecular sunscreen emulsion.

2. The macromolecular sunscreen lotion according to claim 1, characterized in that, The emulsifier is at least two of glyceryl stearate, PEG-100 stearate, cetearyl olive oil ester, sorbitan olive oil ester, arachidonic acid glucoside, and cetyl phosphate potassium, and the mass percentages of glyceryl stearate, PEG-100 stearate, cetearyl olive oil ester, sorbitan olive oil ester, arachidonic acid glucoside, and cetyl phosphate potassium in the macromolecular sunscreen emulsion are 0-2%, 0-2%, 0-2.7%, 0-1.8%, 0-0.5%, and 0.2%-1.5%, respectively.

3. The macromolecular sunscreen lotion according to claim 1, characterized in that, The emulsifying stabilizer is at least two of cetearyl alcohol, arachidyl alcohol, behenyl alcohol, hydrogenated castor oil, and dextrin palmitate, and the mass percentages of cetearyl alcohol, arachidyl alcohol, behenyl alcohol, hydrogenated castor oil, and dextrin palmitate in the macromolecular sunscreen emulsion are 0-1.5%, 0-1.8%, 0-1%, 0-2%, and 0-0.5%, respectively.

4. The macromolecular sunscreen lotion according to claim 1, characterized in that, The skin feel modifier is at least two of polydimethylsiloxane, silica, and polymethylsilsesquioxane, and the mass percentages of polydimethylsiloxane, silica, and polymethylsilsesquioxane in the macromolecular sunscreen are 0%–4%, 0%–1%, and 0%–2%, respectively.

5. The macromolecular sunscreen lotion according to claim 1, characterized in that, The humectant is at least one of dipropylene glycol, 1,3-propanediol, and butylene glycol.

6. The macromolecular sunscreen lotion according to claim 1, characterized in that, The chelating agent is at least one of disodium EDTA and tetrasodium glutamate diacetate.

7. A macromolecular sunscreen lotion, characterized in that, The product comprises the following components by weight percentage: oil-phase sunscreen 7.5%–15.5%, aqueous-phase sunscreen 3%–6%, oil-soluble powder 8%–15%, emulsifier 2%–5%, emulsion stabilizer 1%–3.5%, thickener 0.4%–1.5%, skin feel modifier 2%–6%, moisturizer 6%–10%, chelating agent 0.02%–0.1%, active ingredient 0.3%–3%, preservative 0.8%–1.5%, and water to 100%. Among them, the molecular weight of oil-phase sunscreen agents is greater than 500 Da; The dissolved oils are at least two of the following: butylene glycol dioctanoate / didecanoate, neopentyl glycol diheptanoate, dibutyl adipate, C12-15 benzoate, and diisopropyl sebacate, and the mass percentages of butylene glycol dioctanoate / didecanoate, neopentyl glycol diheptanoate, dibutyl adipate, C12-15 benzoate, and diisopropyl sebacate in the macromolecular sunscreen are 0%–10%, 0–10%, 0–8%, 0–10%, and 0–8%, respectively. The thickener is at least one of xanthan gum, sodium polyacrylamide dimethyl taurate, ammonium polyacrylamide dimethyl taurate, and hydroxyethyl cellulose; The oil-phase sunscreen agent is at least three of the following: diethylhexylbutamidotriazinone, ethylhexyltriazinone, bis-ethylhexyloxyphenol methoxyphenyltriazine, cresoltrazolium trisiloxane, and polysiloxane-15, and the mass percentages of diethylhexylbutamidotriazinone, ethylhexyltriazinone, bis-ethylhexyloxyphenol methoxyphenyltriazine, cresoltrazolium trisiloxane, and polysiloxane-15 in the macromolecular sunscreen emulsion are 1%–3%, 2%–3.5%, 2%–3%, 0%–4%, and 0–2.5%, respectively. The aqueous sunscreen contains (1) terephthalic dimethylene camphor sulfonic acid or its salts, which account for 0.5% to 1% of the mass of the macromolecular sunscreen emulsion; and (2) methylene bis-benzotriazolyl tetramethyl butylphenol, which account for 2.5% to 5% of the mass of the macromolecular sunscreen emulsion.

8. A macromolecular sunscreen lotion, characterized in that, The product comprises the following components by weight percentage: oil-phase sunscreen 7.5%–15.5%, aqueous-phase sunscreen 3%–6%, oil-soluble powder 8%–15%, emulsifier 2%–5%, emulsion stabilizer 1%–3.5%, thickener 0.4%–1.5%, skin feel modifier 2%–6%, moisturizer 6%–10%, chelating agent 0.02%–0.1%, active ingredient 0.3%–3%, fragrance 0.05%–0.3%, and water to 100%. Among them, the molecular weight of oil-phase sunscreen agents is greater than 500 Da; The dissolved oils are at least two of the following: butylene glycol dioctanoate / didecanoate, neopentyl glycol diheptanoate, dibutyl adipate, C12-15 benzoate, and diisopropyl sebacate, and the mass percentages of butylene glycol dioctanoate / didecanoate, neopentyl glycol diheptanoate, dibutyl adipate, C12-15 benzoate, and diisopropyl sebacate in the macromolecular sunscreen are 0%–10%, 0–10%, 0–8%, 0–10%, and 0–8%, respectively. The thickener is at least one of xanthan gum, sodium polyacrylamide dimethyl taurate, ammonium polyacrylamide dimethyl taurate, and hydroxyethyl cellulose; The oil-phase sunscreen agent is at least three of the following: diethylhexylbutamidotriazinone, ethylhexyltriazinone, bis-ethylhexyloxyphenol methoxyphenyltriazine, cresoltrazolium trisiloxane, and polysiloxane-15, and the mass percentages of diethylhexylbutamidotriazinone, ethylhexyltriazinone, bis-ethylhexyloxyphenol methoxyphenyltriazine, cresoltrazolium trisiloxane, and polysiloxane-15 in the macromolecular sunscreen emulsion are 1%–3%, 2%–3.5%, 2%–3%, 0%–4%, and 0–2.5%, respectively. The aqueous sunscreen contains (1) terephthalic dimethylene camphor sulfonic acid or its salts, which account for 0.5% to 1% of the mass of the macromolecular sunscreen emulsion; and (2) methylene bis-benzotriazolyl tetramethyl butylphenol, which account for 2.5% to 5% of the mass of the macromolecular sunscreen emulsion.

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