Modified titanium dioxide for cosmetic use and process for its preparation

Abstract

This invention relates to the field of daily chemical technology, and in particular to a modified titanium dioxide for use in cosmetics and its preparation method. The raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, isopropoxytitanium triisostearate, silica, and titanium dioxide; and the mass ratio of sodium stearoyl glutamate, isopropoxytitanium triisostearate, silica, and titanium dioxide is (2-4):(0.2-1):(1-3):(93-97). Through the synergistic modification of sodium stearoyl glutamate and isopropoxytitanium triisostearate, the surface of the titanium dioxide simultaneously possesses hydrophilicity and lipophilicity, endowing it with excellent interfacial wetting properties. The modified titanium dioxide exhibits good dispersibility and stability in wax-based cosmetic cream systems, silicone oil systems, synthetic ester oil systems, and oil-in-water (O / W) systems, without being limited by the polarity of the oil phase, significantly improving formulation compatibility and adaptability. Furthermore, the titanium dioxide treated by this method effectively combats dullness.

Description

Technical Field

[0001] This invention relates to the field of daily chemical technology, and in particular to a modified titanium dioxide for use in color cosmetics and its preparation method. Background Technology

[0002] Titanium dioxide, a commonly used inorganic pigment, possesses excellent hiding power, dispersibility, and light reflection properties, and is widely used in various cosmetic systems such as makeup, foundation, sunscreen, cushion compacts, and primers. However, titanium dioxide has a strong hydrophilic surface, making it prone to aggregation and difficult to disperse in hydrophobic oil phases or silicone oil systems. Therefore, its surface usually requires oleophilic or hydrophobic modification treatment to improve its stability and skin feel in different cosmetic systems.

[0003] Currently, the two most common modification methods in the industry include:

[0004] 1. Titanium dioxide treated with octyltriethoxysilane (OTES)

[0005] 2. Amino acid-based surface-treated titanium dioxide (such as sodium stearoyl glutamate)

[0006] However, the application of the two modified titanium dioxides mentioned above in color cosmetics or base makeup products has significant limitations. Specifically, triethoxyoctylsilane-treated titanium dioxide has high hydrophobicity and silicone oil affinity, exhibiting good dispersibility only in systems where volatile silicone oils (such as Cyclopentasiloxane, D5) are the main oil phase. However, when the proportion of synthetic ester oils (such as isooctyl isononanoate, caprylic / capric triglycerides, etc.) in the product is high, this type of titanium dioxide cannot maintain uniform dispersion in the system, and is prone to the phenomenon of "color banding," that is, titanium dioxide migration, powder floating, or uneven color development at the boundary in the system. This dispersion instability is particularly evident in color cosmetic cream products, such as lipsticks, contour sticks, and concealers, which have high powder loading and high viscosity systems, making triethoxyoctylsilane-treated titanium dioxide almost unusable.

[0007] On the other hand, amino acid-treated titanium dioxide contains hydrophilic and polar groups on its surface, such as carboxyl and amino groups, which are suitable for forming good interfacial affinity with polar synthetic oils. Therefore, it has good dispersibility and skin feel in water-in-oil systems or base makeup products with synthetic esters as the main oil phase. However, when this type of powder is used in low-polarity silicone oil systems (such as Dimethicone and Cyclomethicone systems), due to the large difference in polarity between the two, amino acid-treated titanium dioxide is not easily wetted in silicone oil, resulting in difficulty in dispersion, particle agglomeration, and severe powder floating. It cannot form a stable system, leading to a decline in formulation performance and a significant deterioration in makeup effect, especially in liquid foundation, where it is prone to dullness.

[0008] Therefore, current titanium dioxide processing methods suffer from limited system compatibility.

[0009] On the one hand, hydrophobic silane-treated powder is only suitable for volatile silicone oil systems and cannot be adapted to multi-element oil formulations;

[0010] On the other hand, while polar amino acid-treated powder is suitable for synthesizing ester oil phases, it is not compatible with silicone oil.

[0011] In the existing technology, there is a lack of a composite modification method for the surface of titanium dioxide powder that is applicable to multiple oil phase systems (especially compatible with silicone oil and ester mixtures) and has good dispersibility, anti-stripping properties, excellent skin feel, and effective anti-dulling properties. Summary of the Invention

[0012] To solve the above-mentioned technical problems, the present invention provides a modified titanium dioxide for use in color cosmetics. The raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, silica and titanium dioxide; and the mass ratio of sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, silica and titanium dioxide is (2-4):(0.2-1):(1-3):(93-97).

[0013] In one embodiment of the present invention, the mass ratio of sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, silica and titanium dioxide is 3:0.8:2.1:93.7.

[0014] In one embodiment of the present invention, the silica comprises spherical silica.

[0015] As one embodiment of the present invention, the raw materials of the modified titanium dioxide also include silicon elastic powder or spherical polymethylsiloxane powder.

[0016] In one embodiment of the present invention, the titanium dioxide is a hollow polymer microsphere composite titanium dioxide.

[0017] As one embodiment of the present invention, the raw materials for preparing the modified titanium dioxide also include PEG-100 stearate.

[0018] In one embodiment of the present invention, the silica comprises hexamethylene diisocyanate modified silica.

[0019] A second aspect of the present invention provides a method for preparing the modified titanium dioxide for color cosmetics, comprising the following steps:

[0020] (1) Add TiO2 to isopropanol, add triisostearate isopropoxytitanium salt, stir at high speed for 2000 rpm, and let stand at room temperature for 30 min to react.

[0021] (2) Dissolve sodium stearoyl glutamate and PEG-100 stearate in water and then mix them. Add 0.1g NaOH to help dissolve and adjust the pH to 7. After mixing the solution, slowly add the slurry obtained in step (1) into the solution and stir for 45 minutes. Control the temperature not to exceed 40℃.

[0022] (3) After filtration and drying, the powder is dry-mixed with hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder and spherical PMMA, and stirred evenly.

[0023] In one embodiment of the present invention, the modified titanium dioxide has an average particle size D50 of 3 to 8 μm.

[0024] The modified titanium dioxide for color cosmetics described in this invention is applied in the field of color cosmetics.

[0025] By adopting the above technical solution, the present invention has the following beneficial effects:

[0026] Synergistic modification with sodium acylglutamate and triisostearic acid isopropoxytitanium salt imparts both hydrophilicity and lipophilicity to the surface of titanium dioxide, resulting in excellent interfacial wetting properties. The modified titanium dioxide exhibits good dispersibility and stability in wax-based cosmetic oil systems, silicone oil systems, synthetic ester oil systems, and oil-in-water (O / W) systems, unaffected by the polarity of the oil phase, significantly improving formulation compatibility and adaptability.

[0027] Even in makeup or base makeup systems with high powder content (≥30%), the modified titanium dioxide of this invention maintains excellent system stability, without flocculation, agglomeration, sedimentation, or interfacial stratification. Its surface treatment structure effectively reduces electrostatic and van der Waals forces between powders, preventing powder self-agglomeration or migration, thereby avoiding "color banding" or powder separation caused by high powder loading.

[0028] By enhancing the wetting coordination between the powder and colored pigments such as iron oxide and pearl powder through triisostearate isopropoxytitanium salt, titanium dioxide can be evenly and synergistically distributed with pigments in a multiphase system, significantly improving color migration and effectively suppressing common problems in makeup / base products such as "color streaks", "floating powder", "uneven color development" and "dullness", resulting in a natural and delicate makeup effect. Detailed Implementation

[0029] The present invention will be further explained below with reference to specific embodiments.

[0030] A modified titanium dioxide for use in color cosmetics, wherein the raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, triisostearic acid isopropoxy titanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, PEG-100 stearate and hollow polymer microsphere composite titanium dioxide; and the mass ratio is (2-4):(0.2-1):(1-3):(0.5-2):(0.5-1):(93-97).

[0031] In one embodiment of the present invention, the mass ratio of sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, PEG-100 stearate and hollow polymer microsphere composite titanium dioxide is 3:0.8:2.1:0.8:0.6:93.7.

[0032] The raw materials for preparing the hollow polymer microsphere composite titanium dioxide are hollow spherical TiO2 and spherical PMMA, with a mass ratio of 92.9:0.8.

[0033] A method for preparing the modified titanium dioxide for color cosmetics, comprising the following steps:

[0034] (1) Add hollow spherical TiO2 to isopropanol, add triisostearate isopropoxytitanium salt, stir at high speed for 2000 rpm, and let it stand at room temperature for 30 min to react.

[0035] (2) Dissolve sodium stearoyl glutamate and PEG-100 stearate in water and then mix them. Add 0.1g NaOH to help dissolve and adjust the pH to 7. After mixing the solution, slowly add the slurry obtained in step (1) into the solution and stir for 45 minutes. Control the temperature not to exceed 40℃.

[0036] (3) After filtering and drying the product from step (2), mix the powder with hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder and spherical PMMA, and stir until uniform.

[0037] This invention provides an excellent multi-surface modification system with high dispersibility, high compatibility, and multiphase adaptability, exhibiting excellent stability and skin feel in makeup, foundation, and even skincare. Sodium stearoyl glutamate provides good water dispersibility and skin affinity, and can be used as a bio-derived hydrophilic coating layer; triisostearic acid isopropoxytitanium salt, due to its hydrophobic long chain, provides good wetting properties to oils, silicone oils, mineral oils, etc., forming an organic titanium network structure on the titanium dioxide surface, significantly enhancing the wetting and hydrophobicity of the oil phase, and is particularly suitable for synthetic ester / silicone oil and other oil phase systems; silica, as fine-sized amorphous particles with hydroxyl groups on the surface, provides mechanical dispersion stability and anti-caking properties, and can also form a weak charge layer to prevent pigment re-aggregation or sedimentation, improving touch and flowability.

[0038] However, the foundation used had a drawback: it wasn't smooth enough to spread. This was because while silica encapsulation helped prevent clumping and improve the feel, excessive silica (especially coarse particles) could lead to a slightly dry, powdery texture. Therefore, spherical polymethylsiloxane was added to the formula for balance. Meanwhile, titanium dioxide treated with triisostearic acid isopropoxytitanium salt had strong coverage and high reflectivity, but the makeup effect wasn't natural enough, appearing white and highly reflective. Therefore, hollow spherical titanium dioxide was used to improve this. Additionally, sodium stearoyl glutamate, being an anionic surfactant, could cause viscosity instability in the foundation, leading to thinning or clumping after a period of time. Therefore, other surfactants were added to the formula for adjustment, resulting in better performance.

[0039] The present invention also provides a foundation liquid, the raw materials for which are prepared include:

[0040] A1: 0.35 parts trihydroxystearin, 3 parts isohexadecane, 2 parts phytosterol / isostearyl / cetearyl alcohol / stearyl / behenol di-linoleic acid ester, tridecyl alcohol trimellitate mixture (mass ratio 4:6), 4.5 parts C9-12 alkyl, cocoyl alcohol-caprylate / decanoate mixture (mass ratio 9:1), 8 parts undecane, tridecane mixture (mass ratio 3:1), 3 parts isodecanyl neopentanoate, 3 parts hydrogenated polyisobutylene, 1 part diisostearyl malate, 4 parts polyglycerol-6 polyricinoleate, 1 part PEG-30 dihydroxystearate, 2 parts polyglycerol-3 diisostearate, 1 part synthetic wax;

[0041] A2: 12 parts modified titanium dioxide;

[0042] A3: 1.0 part of distearate dimethylammonium lithium montmorillonite;

[0043] Phase B: 5 parts butanediol, 1 part glycerol, 1.5 parts sodium chloride, 2 parts ethanol, 0.6 parts of a mixture of phenoxyethanol and ethylhexylglycerol (mass ratio 1:4), and water to make up to 100 parts.

[0044] The present invention provides a method for preparing the foundation liquid as follows:

[0045] (1) Clean and disinfect the necessary containers and equipment;

[0046] (2) Weigh out the A1 phase completely and heat it in a water bath to 70°C until the solid raw material is completely dissolved;

[0047] (3) Add phase A2 to phase A1 and homogenize at medium speed until the color powder is completely dispersed;

[0048] (4) After the A3 phase is activated, it is directly added to the A1A2 phase and homogeneously dispersed completely.

[0049] (5) Dissolve all raw materials of phase B until transparent and heat to 70°C;

[0050] (6) Slowly pour phase B into phase A and homogenize at medium speed. After pouring all the material, homogenize at high speed for 1 minute.

[0051] The following description is based on specific embodiments.

[0052] Example 1

[0053] This embodiment provides a modified titanium dioxide for use in cosmetics. The raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, PEG-100 stearate, and hollow polymer microsphere composite titanium dioxide; and the mass ratio of sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, PEG-100 stearate, and hollow polymer microsphere composite titanium dioxide is 3:0.8:2.1:0.8:0.6:93.7.

[0054] The raw materials for preparing the hollow polymer microsphere composite titanium dioxide are hollow spherical TiO2 and spherical PMMA, with a mass ratio of 92.9:0.8.

[0055] A method for preparing the modified titanium dioxide for color cosmetics, comprising the following steps:

[0056] (1) Add hollow spherical TiO2 to isopropanol (1g / 10ml), add triisostearate isopropoxytitanium salt, stir at high speed for 2000rpm, and let it stand at room temperature for 30min.

[0057] (2) Dissolve sodium stearoyl glutamate (1g / 100ml) and PEG-100 stearate (1g / 50ml) in water respectively and then mix them. Add 0.1M NaOH to help dissolve and adjust the pH to 7. After mixing the solution, slowly add the slurry obtained in step (1) into the solution and stir for 45 minutes. Control the temperature not to exceed 40℃.

[0058] (3) After filtering and drying the product from step (2), mix the powder with hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder and spherical PMMA, and stir until uniform.

[0059] In this embodiment, the preparation method of the hexamethylene diisocyanate modified silica is as follows:

[0060] (1) Weigh 10g of dried fumed silica and add it to anhydrous isopropanol (200mL). Stir for 30 minutes under high-speed dispersion conditions. Heat to 60℃ under nitrogen protection and maintain stirring.

[0061] (2) Add hexamethylene diisocyanate (HDI) to the system at a ratio of 5 wt% (based on the mass of SiO2); at the same time add 0.1% DBTDL, maintain the temperature at about 70°C, and the reaction time is 4 hours. The entire reaction process is kept in an inert atmosphere to avoid moisture interference.

[0062] (3) After the reaction is complete, cool to room temperature and filter out the solid. Wash several times with anhydrous ethanol or toluene to remove unreacted HDI and byproducts. Place the washed modified powder in a vacuum dryer at 50°C for 12 hours.

[0063] In this embodiment, the hollow spherical titanium dioxide was prepared by the preparation method of Example 1 in patent CN104085918B.

[0064] In this embodiment, the spherical polymethylsiloxane powder is Argan Co., Sil-Pearl 4F08.

[0065] In this embodiment, the spherical PMMA is Kowa Chemicals USA, MP-1451.

[0066] This embodiment also provides a liquid foundation, the raw materials of which include:

[0067] 0.35 parts of trihydroxystearin

[0068] 3 parts of isohexadecane

[0069] Two parts of a mixture of phytosterol / isostearyl / cetearyl / stearyl / behenol di-linoleate and tridecyl trimellitate (mass ratio 4:6).

[0070] C9-12 alkyl, coconut oil alcohol-octanoate / decanoate mixture (mass ratio 9:1) 4.5 parts

[0071] 8 parts of a mixture of undecane and tridecane (mass ratio 3:1)

[0072] 3 parts of isodecanyl valerate

[0073] 3 parts hydrogenated polyisobutylene

[0074] 1 part diisostearyl malate

[0075] 4 parts of polyglycerol-6 polyricinoleate

[0076] 1 part PEG-30 dihydroxystearate

[0077] 2 parts polyglycerol-3 diisostearate

[0078] 1 part synthetic wax

[0079] 12 parts modified titanium dioxide

[0080] 1.0 part distearate dimethylammonium lithium montmorillonite

[0081] 5 parts of butylene glycol

[0082] 1 part glycerin

[0083] 1.5 parts sodium chloride

[0084] 2 parts of ethanol

[0085] 0.6 parts of a mixture of phenoxyethanol and ethylhexylglycerin (mass ratio 1:4)

[0086] Add water to make 100 servings.

[0087] This embodiment provides the following method for preparing the foundation liquid:

[0088] (1) Clean and disinfect the necessary containers and equipment;

[0089] (2) Weigh out the A1 phase completely and heat it in a water bath to 70°C until the solid raw material is completely dissolved;

[0090] (3) Add phase A2 to phase A1 and homogenize at medium speed until the color powder is completely dispersed;

[0091] (4) After the A3 phase is activated, it is directly added to the A1A2 phase and homogeneously dispersed completely.

[0092] (5) Dissolve all raw materials of phase B until transparent and heat to 70°C;

[0093] (6) Slowly pour phase B into phase A and homogenize at medium speed. After pouring all the material, homogenize at high speed for 1 minute.

[0094] Example 2

[0095] This embodiment provides a modified titanium dioxide for use in cosmetics. The raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, and hollow polymer microsphere composite titanium dioxide; and the mass ratio of sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, and hollow polymer microsphere composite titanium dioxide is 3.6:0.8:2.1:0.8:93.7.

[0096] The raw materials for preparing the hollow polymer microsphere composite titanium dioxide are hollow spherical TiO2 and spherical PMMA, with a mass ratio of 92.9:0.8.

[0097] A method for preparing the modified titanium dioxide for color cosmetics, comprising the following steps:

[0098] (1) Add hollow spherical TiO2 to isopropanol (1g / 10ml), add triisostearate isopropoxytitanium salt, stir at high speed for 2000rpm, and let it stand at room temperature for 30min.

[0099] (2) Dissolve sodium stearoyl glutamate (1g / 100ml) in water and mix. Add 0.1M NaOH to help dissolve and adjust the pH to 7. After mixing the solution, slowly drop the slurry obtained in step (1) into the solution and stir for 45 minutes. Control the temperature not to exceed 40℃.

[0100] (3) After filtering and drying the product from step (2), mix the powder with hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder and spherical PMMA, and stir until uniform.

[0101] In this embodiment, the preparation method of the hexamethylene diisocyanate modified silica is as follows:

[0102] (4) Weigh 10g of dried fumed silica and add it to anhydrous isopropanol (200mL). Stir for 30 minutes under high-speed dispersion conditions. Heat to 60℃ under nitrogen protection and maintain stirring.

[0103] (5) Add hexamethylene diisocyanate (HDI) to the system at a ratio of 5 wt% (based on the mass of SiO2); at the same time add 0.1% DBTDL, maintain the temperature at about 70°C, and the reaction time is 4 hours. The entire reaction process is kept in an inert atmosphere to avoid moisture interference.

[0104] (6) After the reaction is complete, cool to room temperature and filter out the solid. Wash several times with anhydrous ethanol or toluene to remove unreacted HDI and byproducts. Place the washed modified powder in a vacuum dryer at 50°C for 12 hours.

[0105] In this embodiment, the hollow spherical titanium dioxide was prepared by the preparation method of Example 1 in patent CN104085918B.

[0106] In this embodiment, the spherical polymethylsiloxane powder is Argan Co., Sil-Pearl 4F08.

[0107] In this embodiment, the spherical PMMA is Kowa Chemicals USA, MP-1451.

[0108] This embodiment also provides a liquid foundation, which is prepared using the same raw materials as in Example 1.

[0109] The preparation method of the foundation liquid provided in this embodiment is the same as that in Embodiment 1.

[0110] Example 3

[0111] This embodiment provides a modified titanium dioxide for use in cosmetics. The raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, silica, spherical polymethylsiloxane powder, PEG-100 stearate, and hollow polymer microsphere composite titanium dioxide; and the mass ratio of sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, silica, spherical polymethylsiloxane powder, PEG-100 stearate, and hollow polymer microsphere composite titanium dioxide is 3:0.8:2.1:0.8:0.6:93.7.

[0112] The raw materials for preparing the hollow polymer microsphere composite titanium dioxide are hollow spherical TiO2 and spherical PMMA, with a mass ratio of 92.9:0.8.

[0113] A method for preparing the modified titanium dioxide for color cosmetics, comprising the following steps:

[0114] (1) Add hollow spherical TiO2 to isopropanol (1g / 10ml), add triisostearate isopropoxytitanium salt, stir at high speed for 2000rpm, and let it stand at room temperature for 30min.

[0115] (2) Dissolve sodium stearoyl glutamate (1g / 100ml) and PEG-100 stearate (1g / 50ml) in water respectively and then mix them. Add 0.1M NaOH to help dissolve and adjust the pH to 7. After mixing the solution, slowly add the slurry obtained in step (1) into the solution and stir for 45 minutes. Control the temperature not to exceed 40℃.

[0116] (3) After filtering and drying the product from step (2), mix the powder with hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder and spherical PMMA, and stir until uniform.

[0117] In this embodiment, the hollow spherical titanium dioxide was prepared by the preparation method of Example 1 in patent CN104085918B.

[0118] In this embodiment, the spherical polymethylsiloxane powder is Argan Co., Sil-Pearl 4F08.

[0119] In this embodiment, the spherical PMMA is Kowa Chemicals USA, MP-1451.

[0120] This embodiment also provides a liquid foundation, which is prepared using the same raw materials as in Example 1.

[0121] The preparation method of the foundation liquid provided in this embodiment is the same as that in Embodiment 1.

[0122] Example 4

[0123] This embodiment provides a modified titanium dioxide for use in cosmetics. The raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, triisostearate isopropoxytitanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, PEG-100 stearate, and titanium dioxide; and the mass ratio of sodium stearoyl glutamate, triisostearate isopropoxytitanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, PEG-100 stearate, and titanium dioxide is 3:0.8:2.1:0.8:0.6:93.7.

[0124] The titanium dioxide is hollow spherical TiO2.

[0125] A method for preparing the modified titanium dioxide for color cosmetics, comprising the following steps:

[0126] (1) Add hollow spherical TiO2 to isopropanol (1g / 10ml), add triisostearate isopropoxytitanium salt, stir at high speed for 2000rpm, and let it stand at room temperature for 30min.

[0127] (2) Dissolve sodium stearoyl glutamate (1g / 100ml) and PEG-100 stearate (1g / 50ml) in water respectively and then mix them. Add 0.1M NaOH to help dissolve and adjust the pH to 7. After mixing the solution, slowly add the slurry obtained in step (1) into the solution and stir for 45 minutes. Control the temperature not to exceed 40℃.

[0128] (3) After filtering and drying the product from step (2), dry mix the powder with hexamethylene diisocyanate modified silica and spherical polymethylsiloxane powder and stir until uniform.

[0129] In this embodiment, the preparation method of the hexamethylene diisocyanate modified silica is as follows:

[0130] (7) Weigh 10g of dried fumed silica and add it to anhydrous isopropanol (200mL). Stir for 30 minutes under high-speed dispersion conditions. Heat to 60℃ under nitrogen protection and maintain stirring.

[0131] (8) Add hexamethylene diisocyanate (HDI) to the system at a ratio of 5 wt% (based on the mass of SiO2); at the same time add 0.1% DBTDL, maintain the temperature at about 70°C, and the reaction time is 4 hours. The entire reaction process is kept in an inert atmosphere to avoid moisture interference.

[0132] (9) After the reaction is complete, cool to room temperature and filter out the solid. Wash several times with anhydrous ethanol or toluene to remove unreacted HDI and byproducts. Place the washed modified powder in a vacuum dryer at 50°C for 12 hours.

[0133] In this embodiment, the hollow spherical titanium dioxide was prepared by the preparation method of Example 1 in patent CN104085918B.

[0134] In this embodiment, the spherical polymethylsiloxane powder is Argan Co., Sil-Pearl 4F08.

[0135] This embodiment also provides a liquid foundation, which is prepared using the same raw materials as in Example 1.

[0136] The preparation method of the foundation liquid provided in this embodiment is the same as that in Embodiment 1.

[0137] Example 5

[0138] This embodiment provides a modified titanium dioxide for use in cosmetics. The raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, hexamethylene diisocyanate modified silica, PEG-100 stearate, and hollow polymer microsphere composite titanium dioxide; and the mass ratio of sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, hexamethylene diisocyanate modified silica, PEG-100 stearate, and hollow polymer microsphere composite titanium dioxide is 3:0.8:2.1:1.4:93.7.

[0139] The raw materials for preparing the hollow polymer microsphere composite titanium dioxide are hollow spherical TiO2 and spherical PMMA, with a mass ratio of 92.9:0.8.

[0140] A method for preparing the modified titanium dioxide for color cosmetics, comprising the following steps:

[0141] (1) Add hollow spherical TiO2 to isopropanol (1g / 10ml), add triisostearate isopropoxytitanium salt, stir at high speed for 2000rpm, and let it stand at room temperature for 30min.

[0142] (2) Dissolve sodium stearoyl glutamate (1g / 100ml) and PEG-100 stearate (1g / 50ml) in water respectively and then mix them. Add 0.1M NaOH to help dissolve and adjust the pH to 7. After mixing the solution, slowly add the slurry obtained in step (1) into the solution and stir for 45 minutes. Control the temperature not to exceed 40℃.

[0143] (3) After filtering and drying the product from step (2), the powder is dry-mixed with hexamethylene diisocyanate modified silica and spherical PMMA and stirred evenly.

[0144] In this embodiment, the preparation method of the hexamethylene diisocyanate modified silica is as follows:

[0145] (10) Weigh 10g of dried fumed silica and add it to anhydrous isopropanol (200mL). Stir for 30 minutes under high-speed dispersion conditions. Heat to 60℃ under nitrogen protection and maintain stirring.

[0146] (11) Add hexamethylene diisocyanate (HDI) to the system at a ratio of 5 wt% (based on the mass of SiO2); at the same time add 0.1% DBTDL, maintain the temperature at about 70°C, and the reaction time is 4 hours. The entire reaction process is kept in an inert atmosphere to avoid moisture interference.

[0147] (12) After the reaction is complete, cool to room temperature and filter out the solid. Wash several times with anhydrous ethanol or toluene to remove unreacted HDI and byproducts. Place the washed modified powder in a vacuum dryer at 50°C for 12 hours.

[0148] In this embodiment, the hollow spherical titanium dioxide was prepared by the preparation method of Example 1 in patent CN104085918B.

[0149] In this embodiment, the spherical PMMA is Kowa Chemicals USA, MP-1451.

[0150] This embodiment also provides a liquid foundation, which is prepared using the same raw materials as in Example 1.

[0151] The preparation method of the foundation liquid provided in this embodiment is the same as that in Embodiment 1.

[0152] Example 6

[0153] The difference between this embodiment and Embodiment 1 is that this embodiment provides a modified titanium dioxide for cosmetics, which is the D-phase functional powder material according to Embodiment 3 of Patent CN116889514A.

[0154] Example 7

[0155] This embodiment provides a modified titanium dioxide for use in cosmetics. The raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, silica, and titanium dioxide; and the mass ratio of sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, silica, and titanium dioxide is 3:0.8:2.1:93.7.

[0156] The titanium dioxide is fumed TiO2, purchased from Hubei Huifu Nanomaterials Co., Ltd., NT-50.

[0157] A method for preparing the modified titanium dioxide for color cosmetics, comprising the following steps:

[0158] (1) Add TiO2 to isopropanol (1g / 10ml), add triisostearate isopropoxytitanium salt, stir at high speed for 2000rpm, and let it stand at room temperature for 30min.

[0159] (2) Dissolve sodium stearoyl glutamate (1g / 100ml) in water and mix. Add 0.1M NaOH to help dissolve and adjust the pH to 7. After mixing the solution, slowly drop the slurry obtained in step (1) into the solution and stir for 45 minutes. Control the temperature not to exceed 40℃.

[0160] (3) After filtering and drying the product from step (2), mix the powder with silica and stir until homogeneous.

[0161] This embodiment also provides a liquid foundation, which is prepared using the same raw materials as in Example 1.

[0162] The preparation method of the foundation liquid provided in this embodiment is the same as that in Embodiment 1.

[0163] Performance testing

[0164] Test 1: 10% of the modified titanium dioxide prepared in Examples 1 to 7 was added to the same silicone oil + synthetic ester mixed oil phase system (Cyclopentasiloxane:C12-15Alkyl Benzoate=1:1). After shearing and stirring for 10 minutes, the wetting, sedimentation and uniformity of the powder in the oil phase were observed.

[0165] Table 1 Test Results of Test 1

[0166]

[0167]

[0168] Test 2: The modified titanium dioxide prepared in Examples 1 to 7 was added to a concealer system containing iron oxide (oil-based formula, total powder content 35%). The film was spread on a black and white contrast substrate using a scraper to observe whether color band shift, local whitening, or other "floating color band" phenomena occurred.

[0169] Table 2 Test Results of Test 2

[0170] Example Color band uniformity Color band phenomenon Example 1 Extremely uniform none Example 2 Slightly better Very slight Example 3 Slightly better There is a slight edge offset. Example 4 Half uniform obvious Example 5 Almost uniform Slightly scattered at the edges Example 6 A large part is uneven Noticeably pale Example 7 A large part is uneven Clear sense of boundaries

[0171] Test 3: Coverage and Soft Focus Effect Test

[0172] Each powder was used in the same liquid foundation system (with the same titanium dioxide content) to make a color emulsion. The emulsion was then stretched onto a standard black and white hiding power test card, and its reflectance value (L value) to a black background was measured using a colorimeter. A micrograph was taken to observe the uniformity of diffuse reflection.

[0173] Table 3 Test Results of Test 3

[0174]

[0175]

[0176] Test 4: Accelerated Stability Test

[0177] The foundation liquids of Examples 1 to 7 were stored in an oven at 45°C for 30 days, and the stability changes of the system were observed, including oil-water separation, powder sedimentation, and color changes.

[0178] Table 4. Test Results of Test 4

[0179] Example Is it layered? Whether it settles Color changes Example 1 no no Stablize Example 2 no Very little sedimentation Stablize Example 3 no Very little sedimentation Slightly lighter Example 4 yes obvious Slightly whitish Example 5 no Very little sedimentation Stablize Example 6 yes obvious grayish-white precipitate Example 7 yes obvious Layered yellowing

[0180] Test 5: Skin Feel Evaluation

[0181] A sensory evaluation panel of 30 female participants (aged 20-40, with a balanced distribution of skin types) conducted user experience tests on the concealer systems prepared in different embodiments. Test samples were numbered and blinded. Each participant applied the sample to their face using the standard amount and scored it according to the following four dimensions:

[0182] Table 5 Rating Dimensions

[0183]

[0184] The results are as follows:

[0185] Table 6 shows the test results for Test 5.

[0186]

[0187] Test 6: Dullness Test

[0188] Comparative Example 1: Titanium dioxide (inci: CI 77492 / triethoxyoctylsilane) encapsulated with triethoxyoctylsilane was added to the foundation in the same proportion instead of the titanium dioxide in Example 1, to obtain Comparative Example 1; both Example 1 and Comparative Example 1 were applied to the left and right faces of volunteers respectively (test environment: indoor, room temperature 28-30 degrees Celsius). After the makeup was applied, photos were taken with a mobile phone, and the condition of the foundation on the face was observed every half hour and compared with the initial photos. The observation point when darkening began to appear visibly was recorded.

[0189] Table 7: Observation time of darkening

[0190]

[0191] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A modified titanium dioxide for use in color cosmetics, characterized in that, The raw materials for preparing the modified titanium dioxide include: sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, PEG-100 stearate, and hollow polymer microspheres composite titanium dioxide; and the mass ratio of sodium stearoyl glutamate, triisostearic acid isopropoxytitanium salt, hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder, PEG-100 stearate, and hollow polymer microspheres composite titanium dioxide is 3:0.8:2.1:0.8:0.6:93.7; The hollow polymer microsphere composite titanium dioxide is prepared from hollow spherical TiO2 and spherical PMMA in a mass ratio of 92.9:0.

8. The preparation method of the hexamethylene diisocyanate modified silica is as follows: (1) Weigh 10 g of dried fumed silica and add it to anhydrous isopropanol. Stir for 30 minutes under high-speed dispersion conditions. Heat to 60°C under nitrogen protection and maintain stirring. (2) Add hexamethylene diisocyanate to the system at a ratio of 5 wt% based on the mass of SiO2; at the same time add 0.1% DBTDL, maintain the temperature at about 70°C, and the reaction time is 4 hours. The entire reaction process is kept in an inert atmosphere to avoid moisture interference. (3) After the reaction is complete, cool to room temperature and filter out the solid; wash with anhydrous ethanol or toluene several times to remove unreacted HDI and byproducts; place the washed modified powder under vacuum at 50°C for 12 hours.

2. The modified titanium dioxide for color cosmetics according to claim 1, characterized in that, It is used in the field of color cosmetics.

3. A method for preparing modified titanium dioxide for color cosmetics as described in claim 1, characterized in that, The steps are as follows: (1) Add hollow spherical TiO2 to isopropanol, add triisostearate isopropoxytitanium salt, stir at high speed for 2000 rpm, and let stand at room temperature for 30 min to react. (2) Sodium stearoyl glutamate and PEG-100 stearate are dissolved in water and then mixed. 0.1g NaOH is added to help dissolve and adjust the pH to 7. After mixing the solution, the slurry obtained in step (1) is slowly added dropwise to the solution and stirred for 45 min. The temperature is controlled not to exceed 40℃. (3) After filtration and drying, the powder is obtained. The powder is then mixed with hexamethylene diisocyanate modified silica, spherical polymethylsiloxane powder and spherical PMMA and stirred until uniform.

4. The preparation method according to claim 3, characterized in that, The modified titanium dioxide has an average particle size D50 of 3~8μm.

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