Preparation Method and Application of Zhushushuang Composition

Abstract

The present invention relates to a preparation method and application of a refreshing aid composition. The polydimethylsiloxane of the present invention can be used as a carrier or matrix to uniformly disperse organic sunscreen agents in cosmetics, thereby improving the sunscreen effect and use experience of the product, and minimizing the direct contact opportunity between irritating organic sunscreen agents and the skin. Further, by utilizing the unique properties of the polyorganosiloxane chain that is prone to form a helical structure and the composite structure of the gel aluminum hydroxide / γ-aluminum oxide blend for embedding and anti-inflammatory and smoothing effects, the contact between organic sunscreen agents with a risk of skin sensitization and inorganic sunscreen agents that are prone to cause an unpleasant astringent feeling on the skin is greatly reduced. Combining with skin-nourishing functional substances, a sunscreen product with a high sun protection factor / long-wave ultraviolet protection index that has a refreshing skin feel and is not easily allergic is formulated, combining both sunscreen and beauty functions.

Description

Technical Field

[0001] The present invention relates to the technical field of daily chemical skin care products, and specifically refers to a preparation method and application of a comfort-enhancing composition that can be used in skin care products. Background Art

[0002] With the improvement of people's living standards, consumers pay more and more attention to outdoor activities. However, while enjoying the sunbath, how to prevent the skin from being damaged by ultraviolet rays is an urgent problem to be solved at present.

[0003] At present, combined sunscreen products of organic synthetic sunscreens and inorganic sunscreens meet the above needs because of their quick effectiveness and acceptable persistence. However, due to the influence of human secretions and light environment, the relative action time of organic sunscreens is short, the skin feeling is sticky and heavy, it is difficult to adapt to high-intensity outdoor activities, and the potential allergy risk to the skin always exists; Inorganic sunscreens mainly based on nano-titanium dioxide and nano-zinc oxide have a long sunscreen time, but their relative effect is inferior to that of organic sunscreens, and the cosmetics market is sensitive to the nano concept in skin care products, with frequent restrictive regulations and different production standards need to be adjusted; In addition, during the preparation process of products containing nano-components, due to the limitation of dispersion conditions, the products are prone to agglomeration and appear granular, showing an unpleasant astringent feeling on the skin. Especially for high sun protection index products, the discomfort after application often makes consumers (especially those with allergic constitutions) extremely distressed.

[0004] To solve the above problems, the industry has explored the use of smooth components such as aluminum starch octenyl succinate, lauroyl lysine, modified mica, cyclopentasiloxane and dimethicone and their compositions as additives for the above organic / inorganic sunscreen skin care products in terms of anti-allergy and improving skin feeling. However, so far, there has still been no sunscreen skin care product with a high sun protection index / long-wave ultraviolet protection index that has a comfortable skin feeling and is not allergic. Summary of the Invention

[0005] The first technical problem to be solved by the present invention is to provide a preparation method of a comfort-enhancing composition that can greatly reduce the irritation of organic sunscreens and the unpleasant astringent feeling of inorganic sunscreens, so as to meet the needs of people with sensitive skin, in view of the current situation of the prior art.

[0006] The second technical problem to be solved by the present invention is to provide an application of the above comfort-enhancing composition, which is used in sunscreen skin care products. The sunscreen skin care products can be efficiently absorbed, have a comfortable skin feeling after application, are not easily allergic, and have a skin-nourishing effect at the same time.

[0007] The third technical problem to be solved by the present invention is to provide a preparation method of the above sunscreen skin care products, in view of the current situation of the prior art.

[0008] The technical solution adopted by the present invention to solve at least one of the above technical problems is as follows:

[0009] A preparation method of a comfort-enhancing composition, comprising the following steps:

[0010] (1) Prepare a superacid catalyst

[0011] After uniformly mixing phosphorus pentoxide and crystalline aluminum sulfate, a superacid catalyst is obtained through calcination;

[0012] (2) Prepare an organic sunscreen dispersant

[0013] Ethylhexyl methoxycinnamate, butyl octyl salicylate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl triazone, and diacid ester are heated and then uniformly mixed with butylated hydroxytoluene to obtain a liquid material A;

[0014] (3) Prepare encapsulated polydimethylsiloxane

[0015] Octamethylcyclotetrasiloxane and the above liquid material A are stirred and mixed to obtain a liquid material B;

[0016] The liquid material B is successively reacted with the superacid catalyst and hexamethyldisiloxane to obtain a finished product liquid of encapsulated polydimethylsiloxane, named liquid material C;

[0017] (4) Prepare a hydrated alumina dispersion slurry

[0018] High-purity sodium aluminum carbonate is reacted with an aqueous sodium hydroxide solution to obtain a hydrated alumina dispersion slurry containing sodium aluminate, named liquid material D;

[0019] (5) Prepare a smooth-type modified inorganic powder

[0020] Nanoscale titanium dioxide and nanoscale zinc oxide are batchwise added to the liquid material D, and a layer of gel Al(OH) 3 is deposited on the surfaces of the nanoscale titanium dioxide and zinc oxide particles. After further post-treatment, a modified nanoscale titanium dioxide / zinc oxide smooth-type inorganic sunscreen powder uniformly loaded with a composite structure of gel aluminum hydroxide / γ-aluminum trioxide fusion is obtained, named powder E;

[0021] (6) Prepare the comfort-enhancing composition

[0022] The powder E is put into the liquid material C, and cetyl PEG / PPG-10 / 1 polydimethylsiloxane and dextrin palmitate are added, and after stirring, the target product comfort-enhancing composition is obtained.

[0023] Preferably, the preparation method of the above comfort-enhancing composition specifically comprises the following steps:

[0024] (1) Prepare a superacid catalyst

[0025] Mix phosphorus pentoxide and crystalline aluminum sulfate, and mix them in a certain proportion (ensuring that the ratio of phosphorus to sulfur in the final product is 1:0.5 - 0.7). Disperse them into fine powder by ultrasonic waves in liquid carbon dioxide, restore to room temperature within 1 hour, and react for at least 5 hours under the condition of rapid stirring; transfer the mixture after the preliminary reaction to a high-temperature furnace, heat it to 150 - 160 °C within 1 hour, dehydrate for 2 hours, then heat it to 850 - 880 °C within 2 hours, and calcine for at least 3 hours to make the mixture react fully and generate a superacid catalyst; let the product cool naturally to room temperature and granulate to obtain micron-sized fine particles;

[0026] (2)Prepare the organic sunscreen dispersant

[0027] Mix ethylhexyl methoxycinnamate, butyl octyl salicylate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and ethylhexyl triazone, disperse them in 1 - 1.5 times the amount of dibasic acid ester, heat to 50 - 60 °C to make the material in a homogeneous state, add 0.5% - 0.8% of antioxidant butylated hydroxytoluene based on the total amount of the material, mix well and set aside to obtain liquid A;

[0028] (3)Prepare the encapsulated polydimethylsiloxane

[0029] Stir and mix 40 - 60 parts by weight of octamethylcyclotetrasiloxane and 30 - 50 parts by weight of the above liquid A for 20 - 30 min to obtain liquid B;

[0030] Add 4 - 5 parts by weight of the above superacid catalyst to liquid B under stirring conditions, control the temperature at 60 - 65 °C and stir and react for 6 - 8 h to obtain the hydroxyl-terminated polydimethylsiloxane encapsulated with organic sunscreen, then add 5 - 10 parts by weight of hexamethyldisiloxane, control the temperature at 60 - 70 °C and stir and react for 2 - 3 h to obtain the crude product liquid of the sunscreen polydimethylsiloxane encapsulation; add 200 - 300 parts by weight of purified water, stir rapidly for 20 - 30 min and then wash, let it stand for 2 - 3 h to separate layers, discard the lower aqueous phase to remove impurities such as the catalyst, and dehydrate the upper material and remove the low-boiling hexamethyldisiloxane at 60 - 70 °C under 0.01 MPa for 1.5 - 3 h to obtain the finished product liquid of the sunscreen encapsulated polydimethylsiloxane, named liquid C;

[0031] (4)Prepare the hydrated alumina dispersion slurry

[0032] Put 5 - 10 parts by weight of high-purity sodium aluminum carbonate white powder (the mass content of aluminum trioxide is 40%) into 50 - 100 parts by weight of sodium hydroxide aqueous solution with a volume concentration of 2% - 5% under stirring conditions, stir and react at 70 - 80 °C for 1 - 2 h until the system is nearly transparent to obtain the hydrated alumina dispersion slurry containing sodium aluminate, named liquid D;

[0033] (5)Preparation of smooth modified inorganic powder

[0034] The liquid D is added in batches with nanometer titanium dioxide and nanometer zinc oxide under the bubbling condition of high-purity carbon dioxide. The nanometer titanium dioxide and zinc oxide particles with gel Al(OH) deposited on the surface 3 are dehydrated, dissociated and homogenized in sequence to obtain the powder E; more specifically:

[0035] Under stirring conditions, 5-10 parts by weight of nanometer titanium dioxide and 3-8 parts by weight of nanometer zinc oxide are added in batches to the above-mentioned hydrated alumina dispersion slurry D. The temperature is controlled at 60-70°C, and high-purity carbon dioxide is bubbled in multiple ways at the bottom of the reactor. The reaction is carried out for 15-20 h to make the pH value of the material reach 7.2-7.5, and a layer of gel Al(OH) 3 is deposited on the surface of the nanometer titanium dioxide and zinc oxide particles to obtain composite particles with micron particle size; after completion, the solution is dehydrated by plate-and-frame filtration, then transported to a colloid mill JML-50 for treatment 3 times, dried in an oven at 90-100°C for 1-2 h, then calcined at 450-550°C for 0.5-1 h, and then shock-dissociated and homogenized by a high-pressure air flow of 0.6-0.9 MPa to obtain a modified micron-sized titanium dioxide / nanometer zinc oxide smooth inorganic sunscreen powder uniformly loaded with a gel aluminum hydroxide / γ-aluminum trioxide fusion composite structure, named powder E;

[0036] (6)Preparation of co-smoothing composition

[0037] 13-28 parts by weight of the above-mentioned smooth modified inorganic sunscreen powder E is dispersed and added to 50-90 parts by weight of the finished sunscreen-attached polydimethylsiloxane liquid C under stirring conditions. 1-3 parts by weight of cetyl PEG / PPG-10 / 1 polydimethylsiloxane is added. After mixing evenly, the temperature is raised to 60-70°C, and the mixture is stirred at a speed of 280-350 rpm for at least 2 h until it becomes a homogeneous high-viscosity state. 0.3-0.5 parts by weight of dextrin palmitate is dispersed and added, and the mixture is stirred at a speed of 80-120 rpm for at least 1 h, and cooled to room temperature to obtain the target product co-smoothing composition.

[0038] Preferably, in step (1), the mass ratio of phosphorus to sulfur of the obtained superacid catalyst is 1:(0.5-0.7).

[0039] Preferably, in step (2), the ethylhexyl methoxycinnamate, butyl octyl salicylate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and ethylhexyl triazone are in a mass ratio of 8:(5-6):(2.5-3):(1.5-2); the dibasic acid ester is a mixture of dibutyl adipate and diisopropyl sebacate, and the mass ratio of dibutyl adipate to diisopropyl sebacate is 6:(5-8).

[0040] Preferably, the refreshing composition comprises the following components:

[0041] Powder E 13 - 28 parts by weight,

[0042] Liquid C 50 - 90 parts by weight,

[0043] Cetyl PEG / PPG - 10 / 1 polydimethylsiloxane 1 - 3 parts by weight,

[0044] Dextrin palmitate 0.3 - 0.5 parts by weight.

[0045] Preferably, the Powder E is obtained by preparing with the following components:

[0046] Liquid D 55 - 110 parts by weight,

[0047] Nanoscale titanium dioxide 5 - 10 parts by weight,

[0048] Nanoscale zinc oxide 3 - 8 parts by weight;

[0049] Among them, the Liquid D is obtained by preparing with the following components:

[0050] High - purity sodium aluminum carbonate (high - purity sodium aluminum carbonate is a white powder, and the mass content of aluminum trioxide converted is 40%) 5 - 10 parts by weight,

[0051] Sodium hydroxide aqueous solution with a volume concentration of 2% - 5% 50 - 100 parts by weight.

[0052] Preferably, the Liquid C is obtained by preparing with the following components:

[0053] Liquid B 70 - 110 parts by weight,

[0054] Superacid catalyst 4 - 5 parts by weight,

[0055] Hexamethyldisiloxane 5 - 10 parts by weight,

[0056] Water 200 - 300 parts by weight;

[0057] Among them, the Liquid B is obtained by preparing with the following components:

[0058] Liquid A 30 - 50 parts by weight,

[0059] Octamethylcyclotetrasiloxane 40 - 60 parts by weight.

[0060] A sunscreen skin care product applied with the above - mentioned refreshing composition, by weight, comprises the following components:

[0061] Refreshing composition 45 - 55 parts,

[0062] 1 to 3 parts of vinyl polydimethylsiloxane / polymethylsiloxane sesquioxane cross-linked polymer,

[0063] 1 to 2 parts of cetyl PEG / PPG-10 / 1 polydimethylsiloxane,

[0064] 2 to 3 parts of diethylamino hydroxybenzoyl hexyl benzoate,

[0065] 2 to 4 parts of triethoxysilane octane,

[0066] 1 to 3 parts of isostearic acid,

[0067] 4 to 7 parts of butanediol,

[0068] 2 to 3 parts of methyl methacrylate cross-linked polymer,

[0069] 1 to 3 parts of dimethyldistearylammonium lithium montmorillonite,

[0070] 1 to 2 parts of triethyl citrate,

[0071] 0.5 to 0.8 parts of VP / hexadecene copolymer,

[0072] 1 to 3 parts of PEG-10 polydimethylsiloxane,

[0073] 0.1 to 0.3 parts of phenoxyethanol,

[0074] 1 to 2 parts of ethylhexylglycerin,

[0075] 1 to 2 parts of 1,3-propanediol,

[0076] 0.3 to 0.6 parts of Magnolia biondii extract,

[0077] 0.1 to 0.3 parts of bisabolol,

[0078] 0.1 to 0.2 parts of dipotassium glycyrrhizinate,

[0079] 0.2 to 0.3 parts of p-hydroxyacetophenone,

[0080] 0.1 to 0.2 parts of ectoine,

[0081] 0.08 to 0.12 parts of xanthan gum,

[0082] 20 to 25 parts of water.

[0083] A preparation method of the above sunscreen skin care product, comprising the following steps:

[0084] (1) Mix vinyl polydimethylsiloxane / polymethylsiloxane sesquisiloxane cross-linked polymer and cetyl PEG / PPG-10 / 1 polydimethylsiloxane by stirring until homogeneous, add diethylamino hydroxybenzoyl hexyl benzoate, and stir at room temperature until homogeneous to obtain oil phase G;

[0085] Stir and mix triethoxysilane, triethyl citrate and isostearic acid, heat up to 60 - 65 °C and stir until miscible to form a liquid state. Add VP / hexadecene copolymer and methyl methacrylate cross-linked polymer in batches, stir and mix for at least 1 h until it becomes a homogeneous thick liquid state, disperse lithium magnesium aluminosilicate in it and stir and mix for at least 2 h until it becomes a homogeneous state, then put it into the comfort-enhancing composition, control the rotation speed at 200 - 300 rpm and stir for at least 3 h until it becomes a homogeneous high-viscosity state to obtain oil phase H;

[0086] (2) Under stirring conditions, add PEG-10 polydimethylsiloxane to two-thirds of the total amount of water, melt it to be semi-transparent, add dipotassium glycyrrhizinate and stir until it becomes nearly transparent, then add phenoxyethanol, ethylhexylglycerin and p-hydroxyacetophenone, heat up to 60 - 70 °C and set aside to obtain aqueous phase I;

[0087] Disperse xanthan gum in 1,3-propanediol and butanediol, stir until it becomes a nearly transparent high-viscosity state, add one-third of the total amount of water, stir evenly, add ectoine, MAGNOLIA BIONDII extract and bisabolol, stir evenly and set aside to obtain aqueous phase J;

[0088] (4) Under stirring conditions, control the temperature at 60 - 75 °C, slowly add aqueous phase I to oil phase H, stir for at least 10 minutes until the system reaches the initial state of a high-viscosity W / O emulsion, then control the rotation speed at 3000 - 5000 rpm and homogenize for at least 15 minutes to obtain a homogeneous, high-gloss, high-viscosity W / O emulsion. Cool it to 35 - 38 °C, under stirring conditions, add aqueous phase J, then control the rotation speed at 3000 - 5000 rpm and homogenize for at least 10 minutes, stir until it becomes a high-gloss homogeneous liquid state, then add oil phase G, control the rotation speed at 300 - 400 rpm and stir for at least 30 minutes to obtain a homogeneous, high-gloss, high-viscosity W / O emulsion, and age for 24 h to obtain the target product, a sunscreen skin care product.

[0089] Compared with the prior art, the advantages of the present invention are as follows: The present invention utilizes the unique properties of the polyorganosiloxane chain that is easy to form a helical structure and the composite structure of gel aluminum hydroxide / γ-aluminum oxide to embed and the anti-inflammatory and smooth properties, greatly reducing the contact between the organic sunscreen that has a sensitization risk to the skin and the inorganic sunscreen that is likely to cause an unpleasant astringent feeling on the skin. Combining with skin-nourishing functional substances, a sunscreen skin care product with a high sun protection factor / long-wave ultraviolet protection index that has a comfortable skin feel and is not easily allergic is formulated, which combines sun protection and beauty.

[0090] The specific mechanism of the present invention is described in detail as follows:

[0091] (1) In organosiloxane compounds, the 3d empty orbital on Si in the Si-O bond forms a dπpπ covalent bond with the non-bonding electron pair of the O atom, resulting in the Si-O bond having partial double-bond character and being relatively active. The bond length of the Si-O bond is relatively long, making the steric hindrance for the rotation of its side groups small and it being easily attacked. The electronegativity difference between Si and O is relatively large, and the Si-O bond has 50% ionic character, making polyorganosiloxane very sensitive to reactions with ionic properties. The bond angle of the Si-O bond is relatively large, making it easy for the Si-O bonds to rotate. Due to the mutual compensation of the dπpπ bonds between Si and O and the mutual compensation of the Si-O dipoles, the polyorganosiloxane chain forms a helical structure, with each spiral ring consisting of about 6 silicon-oxygen chain links, and the methyl groups facing outwards to play a shielding role (see Figure 1 ). During the polymerization process, the specific arrangement of the molecular chains of dimethylsiloxane, the maintenance of the balance between rigidity and flexibility, and the intermolecular forces (such as van der Waals forces, hydrogen bonds, etc.) enable the main chain of polydimethylsiloxane to form more complex three-dimensional structures including helical shapes. Such structures with embedding characteristics make it extremely easy to entrap polar organic compounds with electron cloud shift types and organic compounds containing delocalized π bonds, such as ethylhexyl methoxycinnamate, butyl octyl salicylate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and ethylhexyl triazone, during the further polymerization process. In addition, such organic sunscreens are oil-soluble substances and have a certain chemical compatibility with polydimethylsiloxane. They can be more easily entrapped by polydimethylsiloxane. Polydimethylsiloxane can be used as a carrier or matrix to evenly disperse the organic sunscreen in cosmetics, thereby improving the sun protection effect and user experience of the product and minimizing the direct contact opportunity between the irritating organic sunscreen and the skin.

[0092] (2) Nanoscale titanium dioxide and zinc oxide are used as physical sunscreens in sunscreen cosmetics and have high ultraviolet shielding efficiency. However, due to their small particle size, large specific surface area, and extremely high surface energy, they are very likely to form aggregates, which affects the dispersibility and transparency of the product. At the same time, the electron-hole pairs generated after absorbing ultraviolet light may cause the product to change color and produce odors. The gel aluminum hydroxide / γ-aluminum oxide fusion as a coating material has various beneficial properties for the skin. Its astringency helps reduce the greasiness and discomfort of the skin by absorbing the excess moisture on the skin surface. Its antipruritic effect reduces irritation by binding to the acidic substances on the skin surface and relieves the skin itching symptoms. Its antipruritic effect also plays an anti-inflammatory role by neutralizing the acidic substances on the skin surface and reducing the release of inflammatory mediators.

[0093] When nano-titanium dioxide and zinc oxide are coated with a gel aluminum hydroxide / γ-aluminum oxide blend, the agglomeration of nanoparticles can be reduced, thereby improving their dispersibility in cosmetics. The coating layer can protect the nanoparticles from the influence of the external environment, such as light, humidity, etc., thus enhancing their stability. The astringent, antipruritic, and anti-inflammatory effects of the gel aluminum hydroxide in the blend may help reduce the adverse irritation of the nanoparticles to the skin. Gel aluminum hydroxide has excellent oil-absorbing and moisture-absorbing properties, and can effectively adsorb the oil and sweat on the skin surface, keeping the skin fresh and dry. This property enables cosmetics containing gel aluminum hydroxide to reduce the greasiness of the skin and make the makeup more long-lasting and fresh. Gel aluminum hydroxide can help regulate the viscosity of cosmetics, making their texture lighter, smoother, easier to spread evenly, and without a heavy feeling. This regulatory effect makes the cosmetics smoother when applied, not easily pulling the skin, thereby reducing the irritation and damage to the skin. The particulate structure of gel aluminum hydroxide can increase the smoothness between the skin and the cosmetics, making the application process more relaxed and pleasant. This smooth feeling not only improves the use experience but also helps the uniform distribution of the cosmetics on the skin. Gel aluminum hydroxide is a substance with stable chemical properties, not easily reacting with the skin, and not causing irritation or allergy to the skin. At the same time, due to its moderate molecular size, it will not clog pores, further reducing the potential risk to the skin. The framework structure composed of nano-titanium dioxide and zinc oxide coated with a gel aluminum hydroxide / γ-aluminum oxide blend can provide certain support and stability, enabling the pulverized fine powder to form a uniform coating on the skin. This coating can reduce the direct contact area between the titanium dioxide and zinc oxide nanoparticles and the skin, thereby reducing the astringency and other adverse reactions. The smooth-type modified inorganic sunscreen powder containing the gel aluminum hydroxide / γ-aluminum oxide blend composite structure not only maintains excellent physical sunscreen efficacy but also greatly increases the anti-allergic and refreshing properties of the composite powder.

[0094] (3) Nano-titanium dioxide and nano-zinc oxide modified by coating with a gel aluminum hydroxide / γ-aluminum oxide blend can be evenly dispersed in silicone oil to form a stable suspension, which helps reduce the agglomeration and deposition of nanoparticles on the skin, thereby reducing the adverse astringency. Silicone oil has excellent lubricity and compatibility, and can form good interfacial interactions with the coated and modified nanoparticles, helping the formed coating to be more delicate and uniform, better adapting to the skin surface, reducing the friction between the inorganic powder particles and the skin, and further reducing the astringency.

[0095] (4)Magnolia biondii extract, as an active ingredient in cosmetics and skin care products, especially in sun protection and post-sun repair, shows excellent efficacy. Magnolia biondii extract is rich in lignan components, which can provide effective defense before skin sunburn. By targeting and regulating damage-associated molecular patterns (DAMPs) in sunburned cells and inhibiting the release of various cytokines, it can reduce the sensitivity of the skin to ultraviolet rays. After the skin is damaged by ultraviolet rays, Magnolia biondii extract can accelerate the regression of erythema and reduce the skin's inflammatory response. Its soothing and repairing effects help restore the healthy state of the skin. Products containing Magnolia biondii extract, such as sunscreen, spray, gel, etc., can assist in increasing the sun protection factor SPF value and provide more comprehensive protection for the skin. Magnolia biondii extract has a significant soothing effect and can relieve discomfort such as skin flushing and stinging. For sensitive skin, it is a very mild skin care ingredient. Magnolia biondii extract can also be added as an efficacy adjuvant to sun protection and whitening products to enhance the overall effect of the products.

[0096] (5)Ectoin, also known as ectoine or Ectoin, is an amino acid derivative with multiple functions. Ectoin can effectively isolate ultraviolet rays, combat photoaging, and prevent DNA and cell damage caused by ultraviolet rays. It has a significant repair effect on the DNA damage of skin cells caused by ultraviolet ray damage.

[0097] One molecule of ectoin can complex with multiple free water molecules in the skin, structure the free water in skin cells and continuously lock in moisture, thus maintaining the skin osmotic pressure balance. Due to its small molecule size, easy absorption and water solubility, it can significantly increase the skin moisture content. The higher the concentration, the more rapidly the skin moisture content increases. In extreme environments such as high temperature, high salt, and strong ultraviolet rays, ectoin can maintain a good active state and play a protective role for cells. It can also stabilize the structure of enzyme proteins in organisms to ensure the normal operation of molecules inside cells. Ectoin can enhance the immune protection ability of skin cells and increase cell repair ability. It also has strong anti-microbial and anti-allergen capabilities, and at the same time has good anti-allergic and anti-inflammatory functions. Ectoin can enhance the activity of fibroblasts, and then promote the production of hyaluronic acid, collagen and elastic fibers. In short, ectoin is mainly used as an antioxidant and skin conditioner in cosmetics, and has multiple functions such as skin rejuvenation, anti-aging, moisturizing, sun protection, repair, anti-inflammatory and soothing.

[0098] Bisabolol and Dipotassium Glycyrrhizinate are also outstanding in anti-allergic and soothing effects.

[0099] The various skin-nourishing, allergy-relieving and soothing substances of the present invention act synergistically to obtain a sunscreen product with a high sun protection factor / long-wave ultraviolet protection index that has a comfortable skin feel and is non-allergenic. BRIEF DESCRIPTION OF THE DRAWINGS

[0100] Figure 1 It is a structural diagram in the content of the present invention. DETAILED DESCRIPTION OF THE INVENTION

[0101] The present invention will be further described in detail below in conjunction with embodiments.

[0102] Example 1:

[0103] The preparation method of the co-soothing composition in this example is as follows:

[0104] (1) Preparation of superacid catalyst: Mix 5000 grams of phosphorus pentoxide and 6700 grams of anhydrous aluminum sulfate (the ratio of phosphorus to sulfur in the final product is 1:0.6), disperse it into fine powder by ultrasonic wave in liquid carbon dioxide, restore it to room temperature within 1 hour, and react for 6 hours under the condition of fast stirring. Transfer the initially reacted mixture to a high-temperature furnace, heat it to 155 °C within 1 hour, dehydrate for 2 hours, then heat it to 860 °C within 2 hours, and calcine for 3 hours to make the mixture react fully and generate a superacid catalyst. The product is naturally cooled to room temperature and granulated into fine particles of 10 microns.

[0105] (2) Preparation of organic sunscreen dispersant: In a 50-liter stainless steel batching pot with stirring (jacket heating), put 10 kilograms of dibutyl adipate and 10 kilograms of diisopropyl sebacate, stir to form a mixed solution, and respectively put 8 kilograms of ethylhexyl methoxycinnamate, 6 kilograms of butyl octyl salicylate, 2.5 kilograms of bis-ethylhexyloxyphenol methoxyphenyl triazine, and 1.5 kilograms of ethylhexyl triazone as organic sunscreens, stir and mix evenly, heat to 55 °C to make the material in a homogeneous state, add 2.3 kilograms of antioxidant butylated hydroxytoluene, stir well and set aside, named liquid A, with a total of 38 kilograms.

[0106] (3) Preparation of encapsulated polydimethylsiloxane: In a 100-liter high-quality stainless steel batching pot with stirring, put 45 kilograms of octamethylcyclotetrasiloxane and 38 kilograms of the above liquid A, stir and mix for 25 minutes, with a total of 83 kilograms, to obtain liquid B;

[0107] In a 200-liter high-quality stainless steel reaction kettle with stirring (equipped with a large-area condenser and receiver), 83 kg of liquid B was added under stirring conditions (controlled rotation speed of 120 rpm), and then 5 kg of the above-mentioned superacid catalyst was added. The temperature was controlled at 62 °C and stirred for 6 h to obtain hydroxyl-terminated polydimethylsiloxane coated with an organic sunscreen agent. Then, 6 kg of hexamethyldisiloxane was added, and the temperature was controlled at 62 °C and stirred for 3 h to obtain a crude product liquid of sunscreen agent polydimethylsiloxane coating. 100 kg of purified water was added, and it was quickly stirred for 25 min for washing, then allowed to stand for 3 h to separate layers, and the lower aqueous phase was discarded to remove impurities such as catalysts. The upper layer of the material was dehydrated and low-boiling substances were removed at 60 °C under 0.01 MPa for 3 h, and a finished product liquid of sunscreen agent polydimethylsiloxane coating, totaling 88 kg, was obtained, named liquid C.

[0108] (4)Preparation of hydrated alumina dispersion slurry: In a 100-liter high-quality stainless steel reaction kettle with stirring, 60 kg of 3% sodium hydroxide aqueous solution was added, and 8 kg of high-purity sodium aluminum carbonate white powder with 40% aluminum trioxide content was added in three batches. It was stirred at a controlled speed of 80 rpm at 72 °C for 2 h, and the system became almost transparent to obtain 68 kg of hydrated alumina dispersion slurry containing sodium aluminate, named liquid D.

[0109] (5)Preparation of smooth-type modified inorganic powder: In the above-mentioned 100-liter high-quality stainless steel reaction kettle with stirring, under the condition of controlled stirring speed of 180 rpm, 6 kg of nano-titanium dioxide and 4 kg of nano-zinc oxide were added in five batches to the above-mentioned hydrated alumina dispersion slurry liquid D. The temperature was controlled at 60 - 70 °C, and high-purity carbon dioxide was bubbled in from multiple channels at the bottom of the reactor for 18 h to make the pH value of the material reach 7.3, and a gel Al(OH) 3 was deposited on the surface of nano-titanium dioxide and zinc oxide particles to prepare composite particles with a particle size of about 50 microns. After completion, the solution was dehydrated by plate and frame filtration, and then transported to a colloid mill JML-50 for treatment under the action of mechanochemical force. It was dried in an oven at 100 °C for 1 h, then calcined at 500 °C for 0.5 h, and then homogenized by high-pressure air flow impact dissociation at 0.6 MPa to obtain 18 kg of a smooth-type inorganic sunscreen powder with a uniform load of gel aluminum hydroxide / γ-aluminum trioxide fusion composite structure modified nano-titanium dioxide / zinc oxide, named powder E.

[0110] (6)Preparation of the comfort-enhancing composition:

[0111] In a 120-liter high-quality stainless steel reactor with a stirrer, 88 kg of the finished product liquid C wrapped with the sunscreen agent polydimethylsiloxane was put in, and 18 kg of the above-mentioned smooth-type modified inorganic sunscreen powder E was scattered in three batches, stirred evenly, 2 kg of cetyl PEG / PPG-10 / 1 polydimethylsiloxane was added, stirred evenly, then heated to 62 °C, and stirred at a controlled speed of 280 rpm for 3 h until it reached a homogeneous high-viscosity state. 0.4 kg of dextrin palmitate was dispersed and added, stirred at a controlled speed of 100 rpm for 1 h, and cooled to room temperature to obtain a highly effective sunscreen skin care product help-smoothing composition, with a total of 108.5 kg.

[0112] Example 2:

[0113] In this example, the preparation method of the sunscreen skin care lotion is as follows:

[0114] Formula:

[0115] 50 kg of the product help-smoothing composition of Example 1,

[0116] Vinyl polydimethylsiloxane / polymethylsiloxane sesquisiloxane cross-linked polymer 1 kg,

[0117] Cetyl PEG / PPG-10 / 1 polydimethylsiloxane 2 kg,

[0118] Diethylamino hydroxybenzoyl benzoate 3 kg,

[0119] Triethoxysilane 2 kg,

[0120] Isostearic acid 1 kg,

[0121] Butylene glycol 4 kg,

[0122] Methyl methacrylate cross-linked polymer 3 kg,

[0123] Dimethicone diammonium lithium montmorillonite 3 kg,

[0124] Triethyl citrate 2 kg,

[0125] VP / hexadecene copolymer 0.6 kg,

[0126] PEG-10 polydimethylsiloxane 2 kg,

[0127] Phenoxyethanol 0.3 kg,

[0128] Ethylhexylglycerin 2 kg,

[0129] 1,3-propanediol 2 kg,

[0130] Magnolia biondii flower extract 0.6 kg,

[0131] Bisabolol 0.2 kg,

[0132] 0.2 kg of dipotassium glycyrrhizinate,

[0133] 0.3 kg of p-hydroxyacetophenone,

[0134] 0.2 kg of ectoine,

[0135] 0.1 kg of xanthan gum,

[0136] 24 kg of purified water,

[0137] The above materials are all commercially available products, cosmetic grade.

[0138] Process conditions and operation steps:

[0139] (1) In a 10-liter stainless steel batching pot with excellent stirring, add 1 kg of vinyl polydimethylsiloxane / polymethylsiloxane sesquisiloxane cross-linked polymer and 2 kg of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, stir and mix evenly, add 3 kg of diethylamino hydroxybenzoyl benzoate in three batches, and stir and mix evenly at room temperature to obtain oil phase G, with a total of 6 kg.

[0140] In a 15-liter stainless steel batching pot with excellent stirring (jacket heating), add 2 kg of triethoxysilane octane, 2 of triethyl citrate and 1 kg of isostearic acid, mix and heat up to 62 °C, stir and dissolve to form a liquid state, add 3 kg of VP / hexadecene copolymer and methyl methacrylate cross-linked polymer in batches, stir for 1 h to dissolve into a homogeneous thick liquid state, add 3 kg of dimethyldistearylammonium lithium montmorillonite in three batches, stir for 2 h to dissolve into a homogeneous state, and then pump the material into a 100-liter stainless steel batching pot with stirring (jacket heating) containing 50 kg of the high-efficiency sunscreen skin care product help refreshing composition F of Example 1, control the temperature at 62 °C, control the rotation speed at 200 - 300 rpm and stir for 3 h to a homogeneous high-viscosity state to obtain oil phase H, with a total of 61 kg.

[0141] (2) In a 30-liter stainless steel batching pot with excellent stirring (jacket heating), add 16 kg of purified water, add 2 kg of PEG-10 polydimethylsiloxane under stirring conditions to dissolve into a semi-transparent state, add 0.2 of dipotassium glycyrrhizinate and stir to be nearly transparent, add 0.3 kg of phenoxyethanol, 2 kg of ethylhexylglycerin and 0.3 kg of p-hydroxyacetophenone, heat up to 60 - 70 °C for standby to obtain water phase I, with a total of 20.8 kg.

[0142] In a 20-liter premium stirrer (jacket heating) stainless steel batching pot, add 2 kg of 1,3-propanediol and 4 kg of butanediol, stir evenly, add 0.1 kg of xanthan gum in three batches, stir to form an almost transparent high-viscosity state, add 8 kg of purified water, stir evenly, add 0.2 kg of ectoine, 0.6 kg of Magnolia biondii extract and 0.2 kg of bisabolol, stir evenly and set aside to obtain aqueous phase J, totaling 15.1 kg.

[0143] (3) In a 150-liter premium stirrer stainless steel homogenizing and emulsifying pot (equipped with a homogenizer at the bottom), under stirring conditions (controlled rotation speed of 50 rpm), first pump in 61 kg of oil phase H, control the temperature at 70 °C, slowly pump in 20.8 kg of aqueous phase I within 10 minutes, stir for 15 minutes until the initial state of a highly viscous W / O emulsion in the system, then homogenize at a controlled rotation speed of 5000 rpm for 25 minutes to obtain a homogenized, highly shiny and highly viscous W / O emulsion. Cool to 37 °C, under stirring conditions (controlled rotation speed of 100 rpm), pump in 15.1 kg of aqueous phase J, then homogenize at a controlled rotation speed of 3000 rpm for 10 minutes, stir until it becomes a highly shiny homogenized liquid state, then pump in 6 kg of oil phase G, stir at a controlled rotation speed of 300 - 400 rpm for 40 minutes to obtain a homogenized, highly shiny and highly viscous W / O emulsion, and age for 24 hours to obtain the finished product of high-efficiency sunscreen skin care lotion, totaling 103 kg.

[0144] Comparative Example 1:

[0145] Preparation of a physical composition of sunscreen silicone oil:

[0146] Bypass the process of copolymerizing octamethylcyclotetrasiloxane with organic sunscreen agents to produce silicone oil, directly physically blend the organic sunscreen agents with the theoretically calculated amounts of dimethyl silicone oil and carrier esters. At the same time, delete the process of embedding nano-inorganic sunscreen agent particles in the composite structure of gel aluminum hydroxide / γ-aluminum oxide, and directly physically blend the fine powder of aluminum hydroxide with nano-titanium dioxide and nano-zinc oxide. Refer to the formula of Example 1 (scaled down proportionally) to prepare a physical composition of sunscreen silicone oil, which is detailed as follows:

[0147] (1) Preparation of organic sunscreen agent dispersion: In a 50-ml premium stirrer (jacket heating) stainless steel batching cup, add 10 g of dibutyl adipate and 10 g of diisopropyl sebacate, stir to form a mixed solution, add 8 g of ethylhexyl methoxycinnamate, 6 g of butyl octyl salicylate, 2.5 g of bis-ethylhexyloxyphenol methoxyphenyl triazine, and 1.5 g of ethylhexyl triazone as organic sunscreen agents respectively, stir and mix evenly, heat to 55 °C to make the material in a homogeneous state, add 2.3 g of antioxidant butylated hydroxytoluene, stir evenly and set aside, named liquid A, totaling 38 g.

[0148] (2) Preparation of physical blending liquid of organic sunscreen dimethicone: In a 100-ml high-quality stainless-steel batching cup with stirring, 45 g of dimethyl silicone oil and 38 g of the above-mentioned liquid A were put in, and stirred for 25 min to mix, totaling 83 kg to obtain liquid B.

[0149] In a 200-ml high-quality stainless-steel batching cup with stirring, 83 g of liquid B was put in under stirring conditions (controlled rotation speed of 120 rpm), and then 6 g of dimethyl silicone oil was added. The temperature was controlled at 42 °C and stirred for 1 h to obtain the physical blending liquid of organic sunscreen dimethicone, totaling 88 g, named liquid C.

[0150] (3) Preparation of inorganic sunscreen powder of aluminum hydroxide: Cosmetic-grade aluminum hydroxide was processed by a colloid mill JML-50 to prepare fine powder of about 50 microns, and 12 g was weighed, named powder D.

[0151] (5) Preparation of inorganic sunscreen powder containing aluminum hydroxide: 12 g of the above-mentioned micron-sized fine powder of aluminum hydroxide, 6 g of nano-titanium dioxide and 4 g of nano-zinc oxide were transported to a colloid mill JML-50 and mixed under the action of mechanochemical force. It was dried in an oven at 100 °C for 1 h, then calcined at 500 °C for 0.5 h for dehydration, and then homogenized by high-pressure air flow impact dissociation at 0.6 MPa to obtain 18 g of an inorganic sunscreen powder containing aluminum hydroxide with extremely high uniformity, named powder E.

[0152] (6) Preparation of physical composition of sunscreen silicone oil:

[0153] In a 120-ml high-quality stainless-steel reactor with stirring, 88 kg of the physical blending liquid C of organic sunscreen dimethicone was put in, and 18 kg of the above-mentioned inorganic sunscreen powder E containing aluminum hydroxide was scattered in three batches and stirred evenly. 2 g of cetyl PEG / PPG-10 / 1 dimethicone was added, and after stirring evenly, the temperature was raised to 62 °C, and stirred at a controlled rotation speed of 280 rpm for 3 h until it became a homogeneous high-viscosity state. 0.4 g of dextrin palmitate was dispersed and stirred at a controlled rotation speed of 100 rpm for 1 h, and cooled to room temperature to obtain the physical composition of sunscreen silicone oil, totaling 108.5 kg, named physical composition F of sunscreen silicone oil.

[0154] Comparative Example 2:

[0155] Preparation method of sunscreen skin care lotion:

[0156] Replace the co-refreshing composition in the formula of Example 2 with the physical composition F of sunscreen silicone oil in Comparative Example 1, and the formula is as follows:

[0157] 50 g of the physical composition F of sunscreen silicone oil in Comparative Example 1,

[0158] 1 g of vinyl dimethicone / methicone silsesquioxane crosspolymer,

[0159] 2 g of cetyl PEG / PPG-10 / 1 dimethicone,

[0160] 3 g of diethylamino hydroxybenzoyl hexyl benzoate,

[0161] 2 g of triethoxysilane octane,

[0162] 1 g of isostearic acid,

[0163] 4 g of butanediol,

[0164] 3 g of methyl methacrylate crosslinked polymer,

[0165] 3 g of distearyldimonium hectorite,

[0166] 2 g of triethyl citrate,

[0167] 0.6 g of VP / hexadecene copolymer,

[0168] 2 g of PEG-10 dimethicone,

[0169] 0.3 g of phenoxyethanol,

[0170] 2 g of ethylhexylglycerin,

[0171] 2 g of 1,3-propanediol,

[0172] 0.6 g of MAGNOLIA BIONDII flower extract,

[0173] 0.2 g of bisabolol,

[0174] 0.2 g of dipotassium glycyrrhizinate,

[0175] 0.3 g of p-hydroxyacetophenone,

[0176] 0.2 g of ectoine,

[0177] 0.1 g of xanthan gum,

[0178] 24 g of purified water,

[0179] The sunscreen skin care lotion was prepared with reference to the process conditions and operation steps in Example 1.

[0180] The products prepared in Example 2 and Comparative Example 2 of the present invention were subjected to performance testing.

[0181] Evaluation 1. Sunscreen effect test

[0182] Human test on sunscreen effect:

[0183] Sun Protection Factor (SPF): Also known as the Sun Protection Index, it shows the level of sun protection effectiveness that a sun protection product can achieve. The larger the SPF value, the better the sun protection effect. It is determined based on the Minimal Erythema Dose (MED) of the skin. After using a sun protection product, the MED of the skin will increase.

[0184] Sun Protection Factor (SPF): The ratio of the MED required to cause erythema on the skin protected by the sunscreen cosmetic to the MED required to cause erythema on the unprotected skin is the SPF of this sunscreen cosmetic. It can be expressed as follows:

[0185] SPF = MED of the skin protected by the sunscreen cosmetic / MED of the unprotected skin.

[0186] Note: Minimal Erythema Dose (MED) refers to the minimum dose of ultraviolet radiation (J / m 2 ) or the shortest time (seconds) required to cause clearly visible erythema on the skin, and the erythema range reaches most of the irradiated area.

[0187] The SPF index is applicable to evaluating the protection effect against UVB.

[0188] Long-wave Ultraviolet Protection Factor (PFA value) of sunscreen cosmetics: Also known as the UVA protection index. When UVA in sunlight irradiates the skin, it mainly produces the physiological effect of skin darkening, and this effect is measured by the Minimal Persistent Pigment Darkening (MPPD). MPPD is the minimum dose of ultraviolet radiation or the shortest irradiation time required to produce slight pigment darkening on the entire irradiated skin area 2 - 4 hours after irradiation.

[0189] PFA = MPPD of the skin protected by the sunscreen cosmetic / MPPD of the unprotected skin.

[0190] Select the sunscreen skin care lotion of Example 2 and Comparative Example 2, and test the sun protection effect of the product according to the sun protection index test method (human method) of the "Technical Specifications for Cosmetics Safety" (2015 Edition). The test results are shown in Table 1.

[0191] Table 1. Test Results of Sun Protection Effect

[0192] sample SPF PFA Example 2 of the Invention: High-Effect Sunscreen Skin Care Lotion 50.8 16.5 Comparative Example 2: Sunscreen Skin Care Lotion 42.2 11.2

[0193] It can be seen from Table 1 that the highest sun protection index of the high-efficiency sunscreen skin care lotion prepared in Example 2 of the present invention can reach SPF50+ PA+++, and the sun protection index of the sunscreen skin care lotion in Comparative Example 2 is significantly lower compared with that in Example 2.

[0194] Evaluation 2. Skin Comfort and Smoothness

[0195] The basic properties of the high-efficiency sunscreen skin care lotion prepared in Example 2 of the present invention and the sunscreen skin care lotion sample of Comparative Example 2 in terms of skin feel were measured, and the measurement results are shown in Table 2. It can be seen from the test results in Table 2 that the sample of Example 2 of the present invention is superior to Comparative Example 2 in terms of the skin feel smoothness index.

[0196] Table 2. Determination of the core index of skin smoothness

[0197]

[0198] Evaluation 3. Skin stickiness and resistance

[0199] The relevant mechanical data of the combability of the high-efficiency sunscreen skin care lotion of Example 2 of the present invention and the sunscreen skin care lotion of Comparative Example 2 after soaking and drying the hair were tested by the tensile tester method, and their skin stickiness and resistance were indirectly deduced.

[0200] (1) Overview

[0201] The tensile tester is a test instrument specially used for evaluating the hair combing performance. It imitates the human hair combing action through a standard comb, combs a bunch of hair and is recorded by the terminal. When the comb passes through the hair fiber, it shows the force (unit: gf) loaded within a specified displacement (unit: mm) when overcoming the hair resistance and stretching. By detecting the change index of the hair bundle combing force before and after soaking the sample, the aloe glue stickiness is indirectly deduced.

[0202] (2) Materials and methods

[0203] (2.1) Main instruments and materials

[0204] Tensile instrument;

[0205] Thermostatic and humidostatic incubator;

[0206] Several hair bundles: length 50 cm, weight about 16 g;

[0207] Sunscreen skin care lotion: The high-efficiency sunscreen skin care lotion of Example 2 of the present invention and the sunscreen skin care lotion of Comparative Example 2 were both made into 10% water-diluted dispersion dilute emulsion by an ultrasonic dispersion device.

[0208] (2.2) Pretreatment of hair bundles

[0209] Prepare several hair bundles of the same length (50 cm) and weight (about 16 g). First, wash them twice with tap water at 40 °C; then place the hair bundles in a beaker containing 5 g of sodium dodecyl sulfate and 1000 mL of water and heat to 80 °C for soaking; then place the beaker in a thermostatic and humidostatic box at 45 °C for two hours; finally, rinse with tap water until there is no foam and air dry naturally.

[0210] Sample treatment of sunscreen skin care lotion: Weigh 4 g of the diluted and dispersed dilute lotion sample of the sunscreen skin care lotion, rub it onto the treated hair strands until it is in a uniform state, let it stand for 30 minutes, rinse the hair strands with tap water, and blow-dry them with a natural air blower for 30 minutes until they are nearly dry.

[0211] (2.3)Combing property test

[0212] Measure the dry combing property of the hair strands after treatment with the diluted and dispersed dilute lotion sample of the sunscreen skin care lotion on a tensile tester.

[0213] ① Connect the mainframe power supply, turn on the computer, and preheat the instrument for more than half an hour.

[0214] ② Collect all the specimens that make up the test sample together and label each specimen; open the software, create a new sample, select the test method, and name the new sample.

[0215] ③ Comb the hair with a plastic comb first, then fix the hair sample to be tested with a suitable fixture, and place the hair strands naturally in the middle of the comb.

[0216] ④ After completing the calibration and zero adjustment of the instrument, start testing the hair strands. Stretch the hair strands at a speed of 300 mm / min, with a displacement of 200 mm, and take the load value between 100 and 200 mm of displacement. To reduce the measurement error caused by different hair strands, the same hair strand is tested 5 times repeatedly, and the average value is taken (the program automatically records the data and calculates the average value).

[0217] (3)Results and discussion

[0218] This test mainly examines the influence degree of the high-efficiency sunscreen skin care lotion of Example 2 of the present invention and the sunscreen skin care lotion of Comparative Example 2 on the combing property of hair. By testing with a tensile tester and recording the average load value (gf) of the hair strands after treatment with the diluted and dispersed dilute lotion samples of the two sunscreen skin care lotions, the dry hair combing force is compared. The data results are shown in Table 3.

[0219] Table 3

[0220]

[0221] It can be seen from Table 3 that the average dry comb load value (gf) of the hair after treatment with the sunscreen skin care lotion of Example 2 of the present invention is significantly smaller than that of the sunscreen skin care lotion of Comparative Example 2, indirectly indicating that the sticky and obstructive force of the product of the present invention after being applied to the skin is extremely small, and the skin has no rough and astringent feeling.

[0222] Evaluation Four. Patch test

[0223] Test substance: Take the sample prepared in Example 2 for patch testing to detect its potential possibility of causing adverse reactions on human skin.

[0224] Subjects: 38 subjects, including 18 males and 20 females, aged 20-40 years old, were selected as volunteers. Standard test method: Use a syringe to take 0.03mL of sample and place it in the drug chamber of the spot test tape. Immediately apply the spot test tape with the sample to the normal skin of the left forearm from the bottom, and press the drug chambers one by one to expel air and evenly distribute the test substance. Mark the test site for observation. The blank control group is for subjects who do not use the product.

[0225] Result analysis: After 24 hours, the patch test tape was removed, and the skin reaction was observed after half an hour, 24 hours, and 48 hours. The results of the skin reaction were recorded and analyzed according to the CTFA guidelines.

[0226] The identification criteria for skin irritation test are shown in Table 4 below.

[0227] Table 4. Skin irritation test identification standard table

[0228]

[0229] The test results are shown in Table 5 below.

[0230] Table 5. Skin irritation test results

[0231]

[0232] It can be seen from Table 5 that the high-efficiency sunscreen skin care lotion prepared in Example 2 of the present invention does not cause irritation and has good safety.

[0233] Evaluation 5. After application, the skin showed improvements in core beauty data such as increased elasticity, fine pores, reduced number and volume of crow's feet, etc.

[0234] The skin elasticity improvement / anti-wrinkle / pore shrinkage / moisturizing indexes of the high-efficiency sunscreen skin care lotion of Example 2 of the present invention and the sunscreen skin care lotion of Comparative Example 2 were compared and tested using a testing instrument (VISIA-CR Corneometer CM825 Cutometer MPA585 Primos), as shown in Table 6 for details.

[0235] Table 6

[0236]

[0237] Note: For this group of subjects (16 people), the high-efficiency sunscreen skin care lotion of Example 2 of the present invention was used once on the skin on the left side of the face, and at the same time, the sunscreen skin care lotion of Comparative Example 2 was used on the skin on the right side of the face.

[0238] In summary, the embodiment 2 high-efficiency sunscreen skin care lotion of the present invention is significantly superior to the sunscreen skin care lotion of Comparative Example 2 in terms of core data of skin rejuvenation and skin care beauty, such as improved elasticity, finer pores, reduced number of crow's feet, and reduced volume of crow's feet.

Claims

1. A method for preparing a refreshing composition, characterized in that The following steps are involved: (1) Preparation of super acid catalyst: Phosphorus pentoxide and crystalline aluminum sulfate are mixed in a certain proportion to ensure that the phosphorus-sulfur ratio in the final product is 1:(0.5-0.7), dispersed into fine powder in liquid carbon dioxide by ultrasonic wave, returned to room temperature within 1 hour, and reacted for at least 5 hours under fast stirring conditions; the mixture after the preliminary reaction is transferred to a high temperature furnace, and heated to 150-160°C within 1 hour, dehydrated for 2 hours, and then heated to 850-880°C within 2 hours, and calcined for at least 3 hours to allow the mixture to fully react and generate a super acid catalyst; The product is naturally cooled to room temperature and granulated to obtain micron-sized fine particles; (2) Preparing an organic sunscreen dispersion: heating ethylhexyl methoxycinnamate, butyl octanol salicylate, bis-ethylhexyloxyphenol methoxyphenyl triazine, ethylhexyl triazone, and dibasic acid ester and uniformly mixing with butylated hydroxytoluene to obtain a liquid A; (3) Preparation of coated polydimethylsiloxane: octamethylcyclotetrasiloxane and the above-mentioned liquid A were stirred for 20-30 minutes to obtain liquid B; the above-mentioned superacid catalyst was added to liquid B under stirring conditions, and the temperature was controlled at 60-65°C and stirred for 6-8 hours to obtain terminal hydroxyl polydimethylsiloxane coated with organic sunscreen agent; hexamethyldisiloxane was then added, and the temperature was controlled at 60-70°C and stirred for 2-3 hours to obtain a crude liquid of polydimethylsiloxane coated with sunscreen agent; purified water was added, and the mixture was rapidly stirred for 20-30 minutes and then washed, and the mixture was allowed to stand for 2-3 hours to separate, and the lower aqueous phase was discarded to remove impurities such as the catalyst, and the upper layer was dehydrated and the hexamethyldisiloxane low-boiling products were dehydrated at 0.01 MPa at 60-70°C for 1.5-3 hours to obtain a finished liquid of polydimethylsiloxane coated with sunscreen agent, which was named liquid C; (4) Preparing a hydrated alumina dispersion slurry: reacting high-purity sodium aluminum carbonate with an aqueous sodium hydroxide solution to obtain a hydrated alumina dispersion slurry containing sodium aluminate, which is named as liquid D; (5) Preparation of smooth modified inorganic powder: Under high-purity carbon dioxide bubbling conditions, nano-sized titanium dioxide and nano-sized zinc oxide are added to liquid D in batches, and a layer of gel Al(OH)3 is deposited on the surface of the nano-sized titanium dioxide and zinc oxide particles. After further post-treatment, a modified nano-sized titanium dioxide / zinc oxide smooth inorganic sunscreen powder uniformly loaded with gel aluminum hydroxide / γ-aluminum trioxide fusion is obtained, which is named powder E. The post-treatment process is: dehydration by filter pressing, then conveying to a colloid mill for treatment, drying in an oven at 90-100°C for 1-2 hours, and then roasting at 450-550°C for 0.5-1 hour, and then dissociation and homogenization by impact of a high-pressure airflow of 0.6-0.9 MPa; (6) Preparation of a refreshing composition: Powder E is added to liquid C, and cetyl PEG / PPG-10 / 1 polydimethylsiloxane and dextrin palmitate are added, and the refreshing composition is obtained after stirring.

2. The method for preparing the refreshing composition according to claim 1, characterized in that: In step (2), the mass ratio of ethylhexyl methoxycinnamate, butyl octanol salicylate, bis-ethylhexyloxyphenol methoxyphenyl triazine, and ethylhexyl triazone is 8:(5-6):(2.5-3):(1.5-2).

3. The method for preparing the refreshing composition according to claim 1, characterized in that: In step (2), the dibasic acid ester is a mixture of dibutyl adipate and diisopropyl sebacate, and the mass ratio of dibutyl adipate to diisopropyl sebacate is 6:(5-8).

4. The method for preparing the refreshing composition according to any one of claims 1 to 3, characterized in that: The refreshing composition comprises the following components Powder E 13~28 parts by weight, Liquid C 50~90 parts by weight, 1-3 parts by weight of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, Dextrin palmitate 0.3-0.5 parts by weight.

5. The method for preparing the refreshing composition according to claim 4, characterized in that: The smooth modified inorganic powder E is prepared from the following components: Liquid D 55~110 parts by weight, 5-10 parts by weight of nano-sized titanium dioxide, 3-8 parts by weight of nano zinc oxide; Wherein, the feed liquid D is prepared from the following components: 5-10 parts by weight of high-purity sodium aluminum carbonate, 50 to 100 parts by weight of 2% to 5% sodium hydroxide aqueous solution.

6. The method for preparing the refreshing composition according to claim 4, characterized in that: The feed liquid C is prepared from the following components: Liquid B 70~110 parts by weight, 4 to 5 parts by weight of superacid catalyst, 5-10 parts by weight of hexamethyldisiloxane, 200-300 parts by weight of water; Wherein, feed liquid B is prepared from the following components: Liquid A 30~50 parts by weight, 40-60 parts by weight of octamethylcyclotetrasiloxane.

7. A sunscreen skin care product using the refreshing composition according to any one of claims 1 to 6, characterized in that: According to weight parts, it includes the following components: 45-55 parts of refreshing composition, 1-3 parts of vinyl dimethicone / methylsiloxane silsesquioxane crosspolymer, 1~2 parts of cetyl PEG / PPG-10 / 1 polydimethylsiloxane, 2-3 parts of diethylamino hydroxybenzoyl hexyl benzoate, 2~4 parts of triethoxycaprylylsilane, 1~3 parts of isostearic acid, 4-7 parts of butanediol, 2-3 parts of methyl methacrylate cross-linked polymer, 1-3 parts of disteardimethylammonium hectorite, 1~2 parts of triethyl citrate, VP / hexadecene copolymer 0.5-0.8 parts, PEG-10 polydimethylsiloxane 1~3 parts, Phenoxyethanol 0.1~0.3 parts, 1~2 parts of ethylhexylglycerin, 1,3-propylene glycol 1~2 parts, 0.3~0.6 parts of Flos Miscanthus extract, 0.1~0.3 parts of bisabolol, 0.1~0.2 parts of dipotassium glycyrrhizinate, 0.2~0.3 parts of p-hydroxyacetophenone, 0.1-0.2 parts of tetrahydromethylpyrimidine carboxylic acid, Xanthan gum 0.08~0.12 parts, 20~25 parts of water.

8. A method for preparing the sunscreen skin care product according to claim 7, characterized in that The following steps are involved: (1) Vinyl dimethicone / polymethicone silsesquioxane crosspolymer and cetyl PEG / PPG-10 / 1 dimethicone are mixed and stirred until uniformly mixed, and diethylamino hydroxybenzoyl hexyl benzoate is added, and stirred and mixed until uniformly mixed at room temperature to obtain an oil phase G; Triethoxycaprylylsilane, triethyl citrate and isostearic acid are stirred and mixed and heated to 60-65°C and stirred and mixed to form a liquid state, VP / hexadecene copolymer and methyl methacrylate cross-linked polymer are added in batches and stirred and mixed for at least 1 hour until a homogeneous thick liquid state is formed, dispersing disteardimethylammonium hectorite and stirring and mixing for at least 2 hours until a homogeneous state is formed, and then adding it to the refreshing composition, controlling the rotation speed at 200-300 rpm and stirring for at least 3 hours until a homogeneous high viscosity state is formed, to obtain oil phase H; (2) Add PEG-10 polydimethylsiloxane to two-thirds of the total amount of water under stirring and dissolve until it becomes translucent. Add dipotassium glycyrrhizinate and stir until it becomes nearly transparent. Add phenoxyethanol ethylhexylglycerin and p-hydroxyacetophenone and heat to 60-70°C for use to obtain aqueous phase I. (3) Disperse xanthan gum in 1,3-propylene glycol and butylene glycol, stir until it becomes nearly transparent and highly viscous, add one third of the total amount of water, mix well, add tetrahydromethylpyrimidine carboxylic acid, flos dasyphylla extract and bisabolol, mix well and set aside to obtain aqueous phase J; (4) Under stirring conditions, control the temperature at 60-75°C, slowly add the aqueous phase I into the oil phase H, and stir for at least 10 minutes until the system reaches the initial state of a high-viscosity W / O emulsion. Then control the speed at 3000-5000 rpm for homogenization for at least 15 minutes to obtain a homogenous high-gloss and high-viscosity W / O emulsion. Cool to 35-38°C, add the aqueous phase J under stirring conditions, and then control the speed at 3000-5000 rpm for homogenization for at least 10 minutes until it reaches a high-gloss homogenous emulsion state. Then add the oil phase G, control the speed at 300-400 rpm for stirring for at least 30 minutes, homogenize the high-gloss and high-viscosity W / O emulsion, and age it for 24 hours to obtain the target product, a sunscreen skin care product.

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