A powder with oil control and makeup holding effects for sunscreen products or foundation products, and a preparation method and application thereof
Patent Information
- Application Number
- CN202610901913.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-06-22
- Publication Date
- 2026-11-03
AI Technical Summary
Existing technologies struggle to effectively load active ingredients into sunscreens or base makeup products while simultaneously achieving oil control, leading to powder agglomeration and clogged oil-absorbing channels, thus affecting overall performance.
A three-step method of 'powder dispersion - additive construction - active loading' is adopted. By combining spray drying and high-speed dynamic mixing, liquid actives are uniformly loaded onto the surface of porous powder. Combined with the stepwise introduction of film-forming system and functional additives, a stable film structure is constructed, which enhances the smoothness and hydrophobicity of the powder.
It achieves an orderly combination of various functional components, avoids mutual interference, improves the stability and release efficiency of the powder, ensures the fineness and uniformity of the powder and its skin-feeling adhesion, and enhances the oil control and makeup-holding effect.
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Figure CN123024008A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of cosmetics, and more specifically, relates to a powder with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, as well as its preparation method and application. Background Technology
[0002] Titanium dioxide and silica, as powders with oil-controlling and makeup-holding effects used in sunscreens or base makeup products, have been promoted and applied in the market as particulate raw materials added to sunscreens and other cosmetics. See the following related technologies for details:
[0003] The patent application with publication number CN115212138A is for a composite silica sunscreen powder and its preparation method. It includes silica, nano titanium dioxide, solvent, polydimethylsiloxane, and triethoxyoctylsilane, with the following mass percentages of each component: silica 50-100 parts, nano titanium dioxide 30-50 parts, solvent 100-200 parts, polydimethylsiloxane 1-10 parts, and triethoxyoctylsilane 1-10 parts.
[0004] However, it is difficult to make these particles effectively load active ingredients while also having excellent oil control effects, especially for active ingredients in solution form. This can cause the powders to agglomerate, block the oil absorption channels of silica, and ultimately reduce the overall performance of the powders. Summary of the Invention
[0005] The main objective of this invention is to provide a powder with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, and a method for preparing the same. This invention adopts a three-step method of "powder dispersion - auxiliary agent construction - active loading" to ensure that each functional component is clearly layered and orderly combined to avoid mutual interference. Film-forming aids and functional aids are introduced step by step to build a stable film structure while enhancing additional functions such as powder smoothness and hydrophobicity.
[0006] In addition, the present invention also provides applications of this particle.
[0007] The technical solution of the present invention is as follows:
[0008] A method for preparing a powder with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, comprising the following steps:
[0009] Step 1: Knead titanium dioxide and silica together to obtain a mixed powder;
[0010] Step 2: Mix the vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer and the mixed powder to obtain a pre-dispersion;
[0011] Step 3: Add the film-forming aid and silicone oil to the pre-dispersion so that the film-forming aid and silicone oil coat the pre-dispersion;
[0012] Step 4: Add lauroyl lysine and titanate coupling agent to the mixture obtained in step 3 and knead. After kneading evenly, add triethoxyoctylsilane and continue kneading. Then heat to cure and pulverize.
[0013] Step 5: Add the active cosmetic ingredients to the powder obtained in Step 4 and mix them.
[0014] Step 6: Add the complex of acrylate / polydimethylsiloxane copolymer and 10-hydroxydecanoic acid to the product obtained in step 5 and knead it. After kneading until uniform, heat and cure it. After curing, sieve it and collect the sieved material to obtain a powder with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products.
[0015] In the above-mentioned method for preparing powders with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, the titanium dioxide is 1 to 10 parts by weight; the silica is 80 to 90 parts by weight.
[0016] The titanium dioxide has a particle size of 0.2~0.3μm;
[0017] The silica has a particle size of 6-8 micrometers.
[0018] In the above-mentioned method for preparing powders with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, the vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinking polymer is 5 to 10 parts by weight.
[0019] In the above-mentioned method for preparing powders with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, the film-forming aid is trimethylsiloxysilicate and / or acrylate / polydimethylsiloxane copolymer.
[0020] The film-forming aid is 1-3 parts by weight;
[0021] The silicone oil is 0.1 to 1.0 parts by weight.
[0022] In the above-mentioned method for preparing powders with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, the lauroyl lysine is 1-3 parts by weight; the titanate coupling agent is 1-3 parts by weight; the triethoxyoctylsilane is 1-3 parts by weight; the acrylate / polydimethylsiloxane copolymer is 0.01-0.2 parts by weight; and the 10-hydroxydecanoic acid is 0.0005-0.01 parts by weight.
[0023] In the above-mentioned method for preparing powder with oil-controlling and makeup-holding effects for sunscreen products or base makeup products, the particle size of the powder with oil-controlling and makeup-holding effects for sunscreen products or base makeup products is 10~15μm.
[0024] In the above-mentioned method for preparing powders with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, the cosmetic active ingredient is one or more combinations of ceramide, edelweiss extract, and 10-hydroxydecanoic acid.
[0025] In the above-mentioned method for preparing powder with oil-controlling and makeup-holding effects for sunscreen products or base makeup products, step 4 is to use an air jet mill for pulverization, and in step 5, the cosmetic active ingredients are sprayed onto the powder obtained in step 4 for mixing, and the powder obtained in step 4 is in contact with the cosmetic active ingredients in a fluid dynamic manner.
[0026] The curing temperature in step 4 is 100~110℃, and the curing temperature in step 6 is 45~55℃.
[0027] Meanwhile, the present invention also discloses a powder with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, which is prepared by any of the methods described above.
[0028] Finally, the present invention also discloses a cosmetic containing powder as described above for use in sunscreen products or base makeup products, which has oil-controlling and makeup-holding effects.
[0029] One of the above-described technical solutions of the present invention has at least one of the following advantages or beneficial effects:
[0030] This invention employs a three-step method: powder dispersion, additive construction, and active ingredient loading. This ensures that the functional components are clearly layered and orderly combined, avoiding mutual interference. By combining spray drying with high-speed dynamic mixing, liquid active ingredients are uniformly loaded onto the porous powder surface in the form of microdroplets, improving component stability and release efficiency. The coating stage uses medium-temperature curing at 105℃, while the integration stage uses low-temperature baking at 50℃ for an extended period, balancing the stability of the coating layer with the protection of heat-sensitive active ingredients. The film-forming system and functional additives are introduced step-by-step, constructing a stable film structure while enhancing additional functions such as powder smoothness and hydrophobicity. The synergistic effect of high-shear mixing in a kneader and airflow pulverization ensures fine, uniform powder particles without agglomeration, improving skin feel and adhesion. Attached Figure Description
[0031] The present invention will be further described below with reference to the accompanying drawings and embodiments;
[0032] Figure 1 This is a photograph of the powder from Example 1 after it was prepared according to the application formula and left for 0 hours.
[0033] Figure 2 This is a photograph of the powder from Example 1 after it was prepared into the application formula and left to stand for 8 hours.
[0034] Figure 3 The photo shows the powder from Example 1 after it has been prepared into the application formula and left for 24 hours.
[0035] Figure 4 Photograph of the powder prepared for Comparative Example 1 after application of the formulation and left for 0 hours;
[0036] Figure 5 Photograph of the powder prepared for Comparative Example 1 after application and left for 8 hours;
[0037] Figure 6 Photograph of the powder prepared for Comparative Example 1 after application of the formulation and left for 24 hours;
[0038] Figure 7 Photograph of the powder prepared for Comparative Example 6 after application of the formulation and left for 0 hours;
[0039] Figure 8 Photograph of the powder prepared for Comparative Example 6 after application and left for 8 hours;
[0040] Figure 9 Photograph of the powder prepared for Comparative Example 6 after application of the formulation and left for 24 hours;
[0041] Figures 10 to 15 This is a screenshot of a human body test report after the powder from Example 1 of the present invention was prepared into a foundation. Detailed Implementation
[0042] Embodiments of the present invention are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention.
[0043] Example 1
[0044] Phase 1: Raw material premixing and dispersion
[0045] 1. Main powder dispersion
[0046] The kneading process effectively breaks up powder agglomeration by utilizing the shearing, extrusion, and folding forces, uniformly adhering 4 kg of micron-sized titanium dioxide onto 80.2 kg of porous silica (specific surface area: 200±10 m²). 2 / g, 7±1 micrometers, Jiangsu Baili New Materials Co., Ltd.) surface, to achieve preliminary dispersion and homogenization of materials, to obtain a powder mixture.
[0047] The kneading machine used in the kneading process is a 300L model; kneading parameters: 20 minutes, 36 revolutions per minute.
[0048] 2. Introduction of functional powders
[0049] The above powder mixture was coated with 7.3 kg of vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer;
[0050] The coating process is as follows: kneading machine, model: 300L, bonding parameters: 30 minutes, 36 revolutions / minute.
[0051] Phase Two: Construction of the Additive System
[0052] 1. Construction of film-forming system
[0053] 3 kg of film-forming aid (trimethylsiloxane) and 0.3 kg of silicone oil (MIRASIL CM5 A2, molecular weight: 370.77 g / mol INCI: cyclopentamethoxysiloxane) were premixed evenly to form a composite film-forming aid. The composite film-forming aid was slowly added to the system under low-speed kneading until the powder was completely coated.
[0054] The kneading machine used for the low-speed kneading is a 300L model; kneading parameters: 60 minutes, 24 revolutions per minute.
[0055] 2. Introduction of functional additives
[0056] 1.6 kg of lauroyl lysine and 1.3 kg of titanate coupling agent (triisostearate isopropoxytitanium salt) were added sequentially under low-speed kneading to ensure sufficient dispersion of the additives. Finally, 2 kg of triethoxyoctylsilane was added and kneaded until the system was homogeneous. The hydrophobic layer was then coated by baking at 105°C.
[0057] After baking, the material is pulverized at low speed (600 rpm) using a pulverizer, and then fully dispersed through an airflow device. The working pressure of the airflow device is 0.75 MPa, the speed of the classifying wheel is 20,000 r / min, and the final product particle size is controlled within 10-15 micrometers.
[0058] Phase 3: Integration of Active Ingredients
[0059] 1. Active ingredient premix
[0060] 0.5g of ceramide NP, 0.5g of ceramide NP / neuro-suppressant NG, 1g of edelweiss extract, 0.5g of wheat germ oil, and 5g of organic extractant ethanol were premixed and stirred at high speed to form a homogeneous system, thus obtaining the active ingredient.
[0061] 2. Active ingredient loading
[0062] The premixed active ingredient is atomized into small droplets through a nozzle and then fully mixed with the composite powder which is in a high-speed flow state (equipment name: high-speed mixer, model: SHR-500A, process parameters: 800 rpm). The droplets can instantly contact and coat the surface of the composite powder.
[0063] 3. Polymer Integration
[0064] Finally, add 40g of the acrylate / polydimethylsiloxane copolymer and 0.5g of 10-hydroxydecanoic acid complex, and continue kneading until the overall material is uniform. Kneader model: 300L, kneading parameters: 60 minutes, 36 rpm.
[0065] Phase Four: Curing and Shaping
[0066] 1. Spread the kneaded wet material on a tray and transfer it to a constant temperature vacuum drying equipment (50℃) to complete the solidification of the system and the evaporation of the solvent, thereby obtaining a semi-finished functional powder.
[0067] 2. Finally, a high-frequency vibrating screen (screen mesh size: 200 mesh) is used to select large particles of impurities, and the final product is obtained.
[0068] Example 2
[0069] Phase 1: Raw material premixing and dispersion
[0070] 1. Main powder dispersion
[0071] The kneading process effectively breaks up powder agglomeration by utilizing the shearing, extrusion, and folding forces, uniformly adhering 1 kg of micron-sized titanium dioxide onto 90 kg of porous silica (specific surface area: 200±10 m²). 2 / g, 7±1 micrometers, Jiangsu Baili New Materials Co., Ltd.) surface, to achieve preliminary dispersion and homogenization of materials, to obtain a powder mixture.
[0072] The kneading machine used in the kneading process is a 300L model; kneading parameters: 20 minutes, 36 revolutions per minute.
[0073] 2. Introduction of functional powders
[0074] The above powder mixture was coated with 9 kg of vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer;
[0075] The coating process is as follows: kneading machine, model: 300L, bonding parameters: 30 minutes, 36 revolutions / minute.
[0076] Phase Two: Construction of the Additive System
[0077] 1. Construction of film-forming system
[0078] 2 kg of film-forming aid (trimethylsiloxane silicate) and 0.8 kg of silicone oil (MIRASIL CM5 A2, molecular weight: 370.77 g / mol INCI: cyclopentamethoxysiloxane) were premixed evenly to form a composite film-forming aid. The composite film-forming aid was slowly added to the system under low-speed kneading until the powder was completely coated.
[0079] The kneading machine used for the low-speed kneading is a 300L model; kneading parameters: 60 minutes, 24 revolutions per minute.
[0080] 2. Introduction of functional additives
[0081] 1 kg of lauroyl lysine and 3 kg of titanate coupling agent (triisostearate isopropoxytitanium salt) were added sequentially under low-speed kneading to ensure sufficient dispersion of the additives. Finally, 1 kg of triethoxyoctylsilane was added and kneaded until the system was homogeneous. The hydrophobic layer was then coated by baking at 105°C.
[0082] After baking, the material is pulverized at low speed (600 rpm) using a pulverizer, and then fully dispersed through an airflow device. The working pressure of the airflow device is 0.75 MPa, the speed of the classifying wheel is 20,000 r / min, and the final product particle size is controlled within 10-15 micrometers.
[0083] Phase 3: Integration of Active Ingredients
[0084] 1. Active ingredient premix
[0085] 0.5g of ceramide NP, 0.5g of ceramide NP / neuro-suppressant NG, 1g of edelweiss extract, 0.5g of wheat germ oil, and 5g of organic extractant ethanol were premixed and stirred at high speed to form a homogeneous system, thus obtaining the active ingredient.
[0086] 2. Active ingredient loading
[0087] The premixed active ingredient is atomized into small droplets through a nozzle and then fully mixed with the composite powder which is in a high-speed flow state (equipment name: high-speed mixer, model: SHR-500A, process parameters: 800 rpm). The droplets can instantly contact and coat the surface of the composite powder.
[0088] 3. Polymer Integration
[0089] Finally, add 100g of the acrylate / polydimethylsiloxane copolymer and 2g of 10-hydroxydecanoic acid complex, and continue kneading until the overall material is uniform. Kneader model: 300L, kneading parameters: 60 minutes, 36 rpm.
[0090] Phase Four: Curing and Shaping
[0091] 1. Spread the kneaded wet material on a tray and transfer it to a constant temperature vacuum drying equipment (50℃) to complete the solidification of the system and the evaporation of the solvent, thereby obtaining a semi-finished functional powder.
[0092] 2. Finally, a high-frequency vibrating screen (screen mesh size: 200 mesh) is used to select large particles of impurities, and the final product is obtained.
[0093] Example 3
[0094] Phase 1: Raw material premixing and dispersion
[0095] 1. Main powder dispersion
[0096] The kneading process effectively breaks up powder agglomeration by utilizing the shearing, extrusion, and folding forces, uniformly adhering 10 kg of micron-sized titanium dioxide onto 80 kg of porous silica (specific surface area: 200 ± 10 m²). 2 / g, 7±1 micrometers, Jiangsu Baili New Materials Co., Ltd.) surface, to achieve preliminary dispersion and homogenization of materials, to obtain a powder mixture.
[0097] The kneading machine used in the kneading process is a 300L model; kneading parameters: 20 minutes, 36 revolutions per minute.
[0098] 2. Introduction of functional powders
[0099] The above powder mixture was coated with 5 kg of vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer;
[0100] The coating process is as follows: kneading machine, model: 300L, bonding parameters: 30 minutes, 36 revolutions / minute.
[0101] Phase Two: Construction of the Additive System
[0102] 1. Construction of film-forming system
[0103] 1 kg of film-forming aid (trimethylsiloxane silicate) and 0.2 kg of silicone oil (MIRASIL CM5 A2, molecular weight: 370.77 g / mol INCI: cyclopentamethoxysiloxane) were premixed evenly to form a composite film-forming aid. The composite film-forming aid was slowly added to the system under low-speed kneading until the powder was completely coated.
[0104] The kneading machine used for the low-speed kneading is a 300L model; kneading parameters: 60 minutes, 24 revolutions per minute.
[0105] 2. Introduction of functional additives
[0106] 3 kg of lauroyl lysine and 1 kg of titanate coupling agent (triisostearate isopropoxytitanium salt) were added sequentially under low-speed kneading to ensure sufficient dispersion of the additives. Finally, 2 kg of triethoxyoctylsilane was added and kneaded until the system was homogeneous. The system was then baked at 105°C to cure and coat the hydrophobic layer.
[0107] After baking, the material is pulverized at low speed (600 rpm) using a pulverizer, and then fully dispersed through an airflow device. The working pressure of the airflow device is 0.75 MPa, the speed of the classifying wheel is 20,000 r / min, and the final product particle size is controlled within 10-15 micrometers.
[0108] Phase 3: Integration of Active Ingredients
[0109] 1. Active ingredient premix
[0110] 0.5g of ceramide NP, 0.5g of ceramide NP / neuro-suppressant NG, 1g of edelweiss extract, 0.5g of wheat germ oil, and 5g of organic extractant ethanol were premixed and stirred at high speed to form a homogeneous system, thus obtaining the active ingredient.
[0111] 2. Active ingredient loading
[0112] The premixed active ingredient is atomized into small droplets through a nozzle and then fully mixed with the composite powder which is in a high-speed flow state (equipment name: high-speed mixer, model: SHR-500A, process parameters: 800 rpm). The droplets can instantly contact and coat the surface of the composite powder.
[0113] 3. Polymer Integration
[0114] Finally, add 200g of the acrylate / polydimethylsiloxane copolymer and 10g of 10-hydroxydecanoic acid complex, and continue kneading until the overall material is uniform. Kneader model: 300L, kneading parameters: 60 minutes, 36 rpm.
[0115] Phase Four: Curing and Shaping
[0116] 1. Spread the kneaded wet material on a tray and transfer it to a constant temperature vacuum drying equipment (50℃) to complete the solidification of the system and the evaporation of the solvent, thereby obtaining a semi-finished functional powder.
[0117] 2. Finally, a high-frequency vibrating screen (screen mesh size: 200 mesh) is used to select large particles of impurities, and the final product is obtained.
[0118] Comparative Example 1
[0119] Generally the same as Example 1, except that:
[0120] In stage one, the resulting powder mixture is directly subjected to stage two without being coated with vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer.
[0121] The specific process is as follows:
[0122] Phase 1: Raw material premixing and dispersion
[0123] 1. Main powder dispersion
[0124] The kneading process effectively breaks up powder agglomeration by utilizing the shearing, extrusion, and folding forces, uniformly adhering 4 kg of micron-sized titanium dioxide onto 80.2 kg of porous silica (specific surface area: 200±10 m²). 2 / g, 7±1 micrometers, Jiangsu Baili New Materials Co., Ltd.) surface, to achieve preliminary dispersion and homogenization of materials, to obtain a powder mixture.
[0125] The kneading machine used in the kneading process is a 300L model; kneading parameters: 20 minutes, 36 revolutions per minute.
[0126] Phase Two: Construction of the Additive System
[0127] 1. Construction of film-forming system
[0128] 3 kg of film-forming aid (trimethylsiloxane) and 0.3 kg of silicone oil (MIRASIL CM5 A2, molecular weight: 370.77 g / mol INCI: cyclopentamethoxysiloxane) were premixed evenly to form a composite film-forming aid. The composite film-forming aid was slowly added to the system under low-speed kneading until the powder was completely coated.
[0129] The kneading machine used for the low-speed kneading is a 300L model; kneading parameters: 60 minutes, 24 revolutions per minute.
[0130] 2. Introduction of functional additives
[0131] 1.6 kg of lauroyl lysine and 1.3 kg of titanate coupling agent (triisostearate isopropoxytitanium salt) were added sequentially under low-speed kneading to ensure sufficient dispersion of the additives. Finally, 2 kg of triethoxyoctylsilane was added and kneaded until the system was homogeneous. The hydrophobic layer was then coated by baking at 105°C.
[0132] After baking, the material is pulverized at low speed (600 rpm) using a pulverizer, and then fully dispersed through an airflow device. The working pressure of the airflow device is 0.75 MPa, the speed of the classifying wheel is 20,000 r / min, and the final product particle size is controlled within 10-15 micrometers.
[0133] Phase 3: Integration of Active Ingredients
[0134] 1. Active ingredient premix
[0135] 0.5g of ceramide NP, 0.5g of ceramide NP / neuro-suppressant NG, 1g of edelweiss extract, 0.5g of wheat germ oil, and 5g of organic extractant ethanol were premixed and stirred at high speed to form a homogeneous system, thus obtaining the active ingredient.
[0136] 2. Active ingredient loading
[0137] The premixed active ingredient is atomized into small droplets through a nozzle and then fully mixed with the composite powder which is in a high-speed flow state (equipment name: high-speed mixer, model: SHR-500A, process parameters: 800 rpm). The droplets can instantly contact and coat the surface of the composite powder.
[0138] 3. Polymer Integration
[0139] Finally, add 40g of the acrylate / polydimethylsiloxane copolymer and 0.5g of 10-hydroxydecanoic acid complex, and continue kneading until the overall material is uniform. Kneader model: 300L, kneading parameters: 60 minutes, 36 rpm.
[0140] Phase Four: Curing and Shaping
[0141] 1. Spread the kneaded wet material on a tray and transfer it to a constant temperature vacuum drying equipment (50℃) to complete the solidification of the system and the evaporation of the solvent, thereby obtaining a semi-finished functional powder.
[0142] 2. Finally, a high-frequency vibrating screen (screen mesh size: 200 mesh) is used to select large particles of impurities, and the final product is obtained.
[0143] Comparative Example 2
[0144] Generally the same as Example 1, except that:
[0145] When introducing functional additives, only lauroyl lysine is used, and the rest is the same as in Example 1.
[0146] Specifically as follows:
[0147] 2.9 kg of lauroyl lysine was added sequentially under low-speed kneading to ensure sufficient dispersion of the additives. Finally, 2 kg of triethoxyoctylsilane was added, and kneading was continued until the system was homogeneous. The system was then baked at 105°C to cure and coat the hydrophobic layer.
[0148] Comparative Example 3
[0149] Generally the same as Example 1, except that:
[0150] When introducing functional additives, only titanate coupling agents are used, and everything else is the same as in Example 1.
[0151] Specifically as follows:
[0152] 2.9 kg of titanate coupling agent (triisostearic acid isopropoxytitanium salt) was added sequentially under low-speed kneading to ensure sufficient dispersion of the additive. Finally, 2 kg of triethoxyoctylsilane was added, and kneading was continued until the system was homogeneous. The hydrophobic layer was then coated and cured by baking at 105°C.
[0153] Comparative Example 4
[0154] Generally the same as Example 1, except that:
[0155] In Phase 2, no functional additives or triethoxyoctylsilane are introduced; the active ingredient is directly loaded, and everything else is the same as in Example 1.
[0156] Specifically as follows:
[0157] 1.6 kg of lauroyl lysine and 1.3 kg of titanate coupling agent (triisostearate isopropoxytitanium salt) were added sequentially under low-speed kneading conditions to ensure that the additives were fully dispersed and kneaded until the system was homogeneous. The mixture was then baked at 105°C to cure and coat a hydrophobic layer.
[0158] Comparative Example 5
[0159] Generally the same as Example 1, except that:
[0160] In stage two, no film-forming aids are used; instead, lauroyl lysine and titanate coupling agent are added directly, and the rest is the same as in Example 1.
[0161] Comparative Example 6
[0162] Generally the same as Example 1, except that:
[0163] In the active ingredient loading step, the mixing process is carried out in a stirred tank, and the active ingredient is added to the composite powder by spraying.
[0164] Performance testing
[0165] The tests included oil absorption and color stability after placement;
[0166] The testing method is as follows:
[0167] Oil absorption value test method:
[0168] Fill the oleic acid into the burette and record the initial reading V0 (mL).
[0169] Initial rapid dripping: First, rapidly drip oil and acid while pressing, grinding, and stirring with a scraper to allow the oil to quickly soak into the silica powder and prevent clumping.
[0170] Slow dripping in the middle stage: After adding 3 / 4 of the estimated oil absorption, switch to adding drop by drop, and each drop must be fully crushed and scraped to ensure that the oil powder is completely mixed and there is no dry powder.
[0171] Determining the destination (most crucial)
[0172] Continue adding and repeatedly crushing until:
[0173] The entire mixture becomes a uniform, fine, non-loose, non-sticky paste;
[0174] No dry powder, no free oil, no dripping, and no sticking to the scraper;
[0175] Add just one more drop and it will become oily, sticky, and runny—the previous state is the end point.
[0176] Stop adding water and record the final reading of the burette, V1 (mL).
[0177] Result Calculation
[0178] Mass method (g / 100g)
[0179] Oil absorption value = [(V1 − V0) × ρ / m] × 100
[0180] ρ: Oleic acid density (0.89 g / mL, 25℃)
[0181] Color stability after placement: During the above oil absorption test, the changes in color were observed after 8 hours and 24 hours.
[0182] The test results are shown in Table 1.
[0183] Table 1 Test Results
[0184] Oil absorption value / g / 100g 0h 8h 24h Example 1 72.5 Figure 1 Figure 2 Figure 3 Example 2 73.9 / / / Example 3 76.1 / / / Comparative Example 1 69.0 Figure 4 Figure 5 Figure 6 Comparative Example 2 66.6 / / / Comparative Example 3 64.3 / / / Comparative Example 4 60.9 / / / Comparative Example 5 54.8 / / / Comparative Example 6 69.2 Figure 7 Figure 8 Figure 9
[0185] Results analysis:
[0186] 1. As can be seen from Examples 1-3, the powder prepared by the three-step method of "powder dispersion - additive construction - active loading" of the present invention has a high oil absorption value, a stable film structure, and good hydrophobicity;
[0187] 2. As can be seen from Comparative Examples 1 and 5, the simultaneous and reasonable use of film-forming aids and vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymers has a significant impact on the oil absorption value.
[0188] 3. As can be seen from Comparative Examples 2-4, all three functional additives are indispensable, and their influence on oil absorption value is quite significant;
[0189] As can be seen from Example 1 and Comparative Example 6, the flow pattern and velocity of the particles during active ingredient spraying have a certain impact on the oil absorption value, but this impact is the weakest among all factors; however, correspondingly, the discoloration is more obvious after being left for a longer period of time. Figures 1 to 9 It is evident that the combination and matching of the various factors in this invention are also crucial for maintaining placement stability.
[0190] Human experimentation
[0191] The sample from Example 1 was prepared into a foundation and sent for external testing (Dierxi (Guangzhou) Testing Technology Co., Ltd., Report No.: 2026GX043YP01B01).
[0192] The formula and process are shown in Table 2:
[0193] Table 2 Formulation and Process
[0194] Test methods and results reference Figures 10 to 15 ;
[0195] Tests show that the product of this invention has good oil control, skin feel, and makeup-holding effect.
Claims
1. A method for preparing a powder with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, characterized in that, Includes the following steps: Step 1: Knead titanium dioxide and silica together to obtain a mixed powder; Step 2: Mix the vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinked polymer and the mixed powder to obtain a pre-dispersion; Step 3: Add the film-forming aid and silicone oil to the pre-dispersion so that the film-forming aid and silicone oil coat the pre-dispersion; Step 4: Add lauroyl lysine and titanate coupling agent to the mixture obtained in step 3 and knead. After kneading evenly, add triethoxyoctylsilane and continue kneading. Then heat to cure and pulverize. Step 5: Add the active cosmetic ingredients to the powder obtained in Step 4 and mix them. Step 6: Add the complex of acrylate / polydimethylsiloxane copolymer and 10-hydroxydecanoic acid to the product obtained in step 5 and knead it. After kneading until uniform, heat and cure it. After solidification, the material is sieved and the sieved material is collected to obtain a powder with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products.
2. The method for preparing powder according to claim 1, characterized in that, The titanium dioxide is 1-10 parts by weight; the silica is 80-90 parts by weight. The titanium dioxide has a particle size of 0.2~0.3μm; The silica has a particle size of 6-8 micrometers.
3. The method for preparing powder according to claim 1, characterized in that, The vinyl polydimethylsiloxane / polymethylsiloxane sesquioxane crosslinked polymer is present in 5-10 parts by weight.
4. The method for preparing powder according to claim 1, characterized in that, The film-forming aid is trimethylsiloxysilicate and / or acrylic (ester) / polydimethylsiloxane copolymer; The film-forming aid is 1-3 parts by weight; The silicone oil is 0.1 to 1.0 parts by weight.
5. The method for preparing powder according to claim 1, characterized in that, The lauroyl lysine is 1-3 parts by weight; the titanate coupling agent is 1-3 parts by weight; the triethoxyoctylsilane is 1-3 parts by weight; the acrylate / polydimethylsiloxane copolymer is 0.01-0.2 parts by weight; and the 10-hydroxydecanoic acid is 0.0005-0.01 parts by weight.
6. The method for preparing powder according to claim 1, characterized in that, The powder used in sunscreen or base makeup products with oil-control and makeup-holding effects has a particle size of 10~15μm.
7. The method for preparing powder according to claim 1, characterized in that, The active ingredient in the cosmetic is one or more of the following: ceramide, edelweiss extract, and 10-hydroxydecanoic acid.
8. The method for preparing powder according to claim 1, characterized in that, In step 4, an air jet mill is used for pulverization. In step 5, the active cosmetic ingredient is sprayed onto the powder obtained in step 4 for mixing. The powder obtained in step 4 comes into contact with the active cosmetic ingredient in a fluid dynamic manner. The curing temperature in step 4 is 100~110℃, and the curing temperature in step 6 is 45~55℃.
9. A powder with oil-controlling and makeup-holding effects for use in sunscreen products or base makeup products, characterized in that, It is prepared by the method described in any one of claims 1 to 8.
10. A cosmetic product, characterized in that, It contains the powder as described in any one of claims 1 to 8.
Citation Information
Patent Citations
Composite silica sunscreen powder and preparation method thereof
CN115212138A
