Method for producing silica particles and their use in cosmetic compositions

Abstract

To provide a personal care formulation that exhibits excellent elongation, feel, and good adhesion to the skin, and causes less makeup collapse, a reduction in soft focus effect that creates uneven skin tones, and a reduction in appearance of uneven skin texture, such as pores and wrinkles.SOLUTION: Provided is a personal care formulation comprising silica particles. The silica particles comprising repeating units of (SiO4 / 2). The silica particles have a D90 / D10 particle size distribution of about 1.3 or less as determined by a particle size analyzer utilizing a laser diffraction particle size analysis. The silica particles are spherical and have a sphericity greater than or equal to 0.9, defined as minor axis / major axis.SELECTED DRAWING: None

Description

Field Technology

[0001] This disclosure describes a spherical particle having a D90 / D10 particle size distribution of approximately 1.3 or less when measured by laser diffraction, and a sphericity of 0.9 or more defined by the short axis / long axis (SiO 4 / 2 This disclosure relates to silica particles containing repeating units of ). The disclosure also relates to personal care compositions containing such silica particles. [Background technology]

[0002] The personal care industry has grown by offering multi-performance products based on mixtures of several ingredients, each possessing important or desirable performance characteristics in the final formulation. Spherical silica microparticles are commonly added to various personal care formulations to enhance the aesthetic aspects related to spreadability and tactile sensation. However, conventional spherical silica microparticles have poor skin adhesion.

[0003] Spherical silica microparticles have been previously proposed for incorporation into personal care formulations. However, the non-uniform particle size of the spherical particles results in unsatisfactory spreadability and feel. Therefore, there is a need to provide personal care formulations that offer superior spreadability, feel, and good adhesion to the skin, less makeup breakdown, reduced soft-focus effect that creates uneven skin tone, and minimize the appearance of uneven skin texture such as pores and wrinkles. [Overview of the project]

[0004] In the first embodiment, this disclosure relates to (SiO 4 / 2 With respect to silica particles containing repeating units of ), where the silica particles have a particle size distribution defined as D90 / D10 of approximately 1.3 or less when measured by a particle size analyzer utilizing laser diffraction, where the silica particles are spherical and have a sphericity of 0.9 or greater, defined by the short axis / long axis.

[0005] In one embodiment, the silica particles have a median particle size (D50) ranging from approximately 0.5 μm to approximately 50 μm.

[0006] In one embodiment, the silica particles are approximately 0.1 m 2 From / g to approximately 100m 2 It has a BET surface area of ​​ / g.

[0007] In one embodiment, the silica particles have a sphericity of 0.95 or higher.

[0008] In one embodiment, the silica particles are non-porous.

[0009] In one embodiment, silica particles are surface-treated with at least one hydrophobic agent. In a further embodiment, the hydrophobic agent is a trialkoxysilane compound. In another embodiment, the hydrophobic agent is hexamethyldisilazane.

[0010] In a further embodiment, the Disclosure provides a method for producing silica particles, the method comprising heating polymethylsilsesquioxane fine particles at a temperature of 500°C or less to form silica particles, wherein the silica particles are spherical and have a sphericity of 0.9 or greater, defined by the short axis / long axis.

[0011] In one embodiment, polymethylsilsesquioxane fine particles are heated in an atmosphere containing approximately 20% or less oxygen.

[0012] In one embodiment, the polymethylsilsesquioxane fine particles are heated for about 10 minutes to about 6 hours.

[0013] In one embodiment, the method further includes lowering the temperature of the polymethylsilsesquioxane fine particles to about 400°C.

[0014] In one embodiment, polymethylsilsesquioxane fine particles are heated in an atmosphere containing approximately 20% or less oxygen.

[0015] In one embodiment, polymethylsilsesquioxane fine particles are heated in an electric furnace, a gas furnace, a far-infrared furnace, a mid-infrared furnace, or a near-infrared furnace.

[0016] In another embodiment, this disclosure relates to silica particles prepared by the method disclosed herein. In a further embodiment, the silica particles have a median (D50) particle size ranging from about 0.5 μm to about 50 μm, as measured by a particle size analyzer utilizing laser diffraction particle size analysis.

[0017] In one embodiment, silica particles, when measured by a particle size analyzer utilizing laser diffraction particle size analysis, have a particle size distribution defined as D90 / D10 of approximately 1.3 or less.

[0018] In one embodiment, the silica particles are spherical with a sphericity of 0.9 or higher.

[0019] In one embodiment, the silica particles are non-porous.

[0020] In one embodiment, the personal care formulation comprises silica particles as described herein. In some embodiments, the composition further comprises preservatives, antioxidants, binders, defoamers, antistatics, colorants, emulsifying stabilizers, oxidizing agents, propellants, opacifiers, UV filters, UV absorbers, modifiers, viscosity modifiers, modifiers, chelating agents, gums or thickeners, oils, waxes, fragrances, essential oils, emulsifiers, surfactants, and combinations thereof. In further embodiments, the personal care is a deodorant, antiperspirant, skin cream, facial cream, hair shampoo, hair conditioner, mousse, hair styling gel, hair spray, protective cream, lipstick, facial foundation, blush, makeup, and mascara, skincare lotion, moisturizer, facial treatment, personal cleanser, facial cleanser, bath oil, perfume, shaving cream, pre-shave lotion, aftershave lotion, cologne, sachet, toothpaste, or sunscreen. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] [Figure 1] Figure 1 is a graph showing that a powder formulation comprising silica having a narrow particle size distribution (D90 / D10=1.1) exhibits a lower coefficient of friction than a formulation having a broader particle size distribution (D90 / D10=1.9).

[0022] [Figure 2] Figure 2 is an image showing measurement of the sphericity (minor axis / major axis) of particles.

[0023] [Figure 3] Figures 3A and 3B are distribution graphs showing the particle size distribution of spherical particles prepared using the method of Example 1 (Figure 3A) and Comparative Example 6 (Figure 3B), respectively. DESCRIPTION OF EMBODIMENTS

[0024] I. Definitions Unless otherwise stated, any atom having an unsatisfied valence is assumed to have sufficient hydrogen atoms to satisfy the valence.

[0025] The singular forms "a", "an", and "the" include plural referents unless the context clearly dictates otherwise.

[0026] Furthermore, when used herein, “and / or” should be interpreted as referring to the specific disclosure of each of two specific features or components, with or without the other. Thus, the term “and / or” as used in phrases such as “A and / or B” herein is intended to include “A and B,” “A or B,” “A” (alone), and “B” (alone). Similarly, the term “and / or” as used in phrases such as “A, B, and / or C” is intended to include each of the following embodiments, namely A, B, and C; A, B, or C; A or C; A or B; B or C; A and C; A and B; B and C; A (alone); B (alone); and C (alone).

[0027] Whenever an aspect is described herein in the language of “comprising,” it is understood that similar aspects are also given in relation to “consisting of” and / or “consisting essentially of.”

[0028] The term "approximately" is used herein to mean roughly, broadly, around, or within a range. When the term "approximately" is used in conjunction with a numerical range, it modifies that range by widening the upper and lower boundaries of the indicated number. Generally, the term "approximately" can change the numbers above and below the stated value by, for example, 10 percent up or down (higher or lower).

[0029] As used in this specification, the term "BET surface area" refers to the Brunauer-Emmett-Teller surface area.

[0030] As used herein, the term "sphericity" refers to a parameter indicating how close a particle is to a perfect sphere, and is defined as the long axis / short axis and short axis / long axis obtained from scanning microscope images of the particle. (See Figure 2)

[0031] As used herein, the following definitions shall apply unless otherwise indicated. For the purposes of this disclosure, chemical elements are identified in accordance with the Periodic Table of Elements, CAS versions, and the Handbook of Chemistry and Physics, 75th edition, 1994. Furthermore, general principles of organic chemistry are found in "Organic Chemistry," Thomas Sorrell, University Science Books, Sausalito: 1999, and "March's Advanced Organic Chemistry," 6th edition, edited by Smith, MB and March, J., John Wiley & Sons, New York: 2007, the entire contents of which are incorporated herein by reference.

[0032] Various aspects of this disclosure are described in more detail below.

[0033] II. Silica particles In one aspect, this disclosure is (SiO 4 / 2 With respect to silica particles containing the units ), where the silica particles, when measured with a particle size analyzer utilizing laser diffraction particle size analysis, have a D90 / D10 particle size distribution of approximately 1.3 or less, where the silica particles are spherical and have a sphericity of 0.9 or greater, defined by the short axis / long axis.

[0034] a. Particle size In some embodiments, the silica particles have a D90 / D10 particle size distribution of about 1.0 to about 1.2. In some embodiments, the silica particles have a D90 / D10 particle size distribution of about 1.0, about 1.1, or about 1.2.

[0035] In some embodiments, the silica particles have a median (D50) particle size of from about 0.5 μm to about 50 μm. In further embodiments, the silica particles have a median (D50) particle size of from about 1 μm to about 20 μm. In another embodiment, the silica particles have a median (D50) particle size of from about 1 μm to about 10 μm. In still another embodiment, the silica particles have a median (D50) particle size of from about 1 μm to about 5 μm. In some embodiments, the silica particles have a median (D50) particle size of about 0.5, about 0.75, about 1, about 1.25, about 1.5, about 1.75, about 2, about 2.25, about 2.5, about 2.75, about 3, about 3.25, about 3.5, about 3.75, about 4, about 4.25, about 4.5, about 4.75, about 5, about 10, about 15, about 20, about 25, about 30, about 35, about 40, about 45, or about 50 μm.

[0036] b. Surface Area In some embodiments, the silica particles have a BET surface area of from about 0.1 m 2 / g to about 100 m 2 / g, as measured by a TriStar II Plus (Micromeritics). In further embodiments, the silica particles have a BET surface area of from about 0.1 m 2 / g to about 90 m 2 / g. In some embodiments, the silica particles have a BET surface area of about 0.1, about 0.25, about 0.5, about 0.75, about 1, about 1.5, about 2, about 2.5, about 3, about 3.5, about 4, about 4, about 4.5, about 5, about 10, about 15, about 20, about 25, about 30, about 35, about 40, about 45, about 50, about 55, about 60, about 65, about 70, about 75, about 80, about 85, about 90, about 95, or about 100 m 2 / g.

[0037] c. Particle Sphericity In some embodiments, the silica particles have a sphericity of 0.95 or higher. In some embodiments, the silica particles have a sphericity of from 0.95 to 1.

[0038] d. Particle Surface In some embodiments, the silica particles are non-porous.

[0039] In some embodiments, the silica particles are surface-treated with at least one hydrophobic agent. In some embodiments, the hydrophobic agent is alkylsilane (e.g., triethoxycaprylylsilane or dimethylsilyl agents), metal soap (e.g., isopropyl titanium triisostearate), stearyl-modified amino acids (e.g., disodium stearoyl glutamate and aluminum hydroxide), silicone (e.g., dimethicone), fluoride (e.g., perfluorooctyltriethoxysilane), and mixtures thereof. In some embodiments, the hydrophobic agent is hexamethyldisilazane.

[0040] III. Method In one embodiment, the disclosure relates to a method for producing silica particles, the method comprising heating polymethylsilsesquioxane fine particles at a temperature of 600°C or less to form silica particles, wherein the silica particles are spherical and have a sphericity of 0.9 or greater, defined by the ratio of the short axis to the long axis.

[0041] i.Temperature In some embodiments, the polymethylsilsesquioxane fine particles are heated to a temperature of about 500°C or less. In further embodiments, the polymethylsilsesquioxane fine particles are heated to a temperature of about 400°C or less.

[0042] In some embodiments, polymethylsilsesquioxane particles are heated in an electric furnace, a gas furnace, a far-infrared furnace, a mid-infrared furnace, or a near-infrared furnace.

[0043] ii. Atmosphere In some embodiments, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 20% or less oxygen. In further embodiments, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 15% or less oxygen. In yet another embodiment, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 10% or less oxygen. In some embodiments, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 20% or less oxygen, about 15% or less oxygen, about 10% or less oxygen, or about 5% or less oxygen. In some embodiments, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 20%, about 15%, about 10%, about 5%, about 4%, about 3%, about 2%, or about 1% oxygen.

[0044] iii. Time In some embodiments, the polymethylsilsesquioxane particles are heated for about 10 minutes to about 6 hours. In further embodiments, the polymethylsilsesquioxane particles are heated for about 30 minutes to about 5 hours. In some embodiments, the polymethylsilsesquioxane particles are heated for about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, about 1 hour, about 1.25 hours, about 1.5 hours, about 1.75 hours, about 2 hours, about 2.25 hours, about 2.5 hours, about 2.75 hours, about 3 hours, about 2.25 hours, about 3.5 hours, about 3.75 hours, about 4 hours, about 4.25 hours, about 4.5 hours, about 4.75 hours, about 5 hours, about 5.25 hours, about 5.5 hours, about 5.75 hours, or about 6 hours.

[0045] b. Optional heating step In some embodiments, the method may further include lowering the temperature of the polymethylsilsesquioxane particles to about 400°C.

[0046] i. atmosphere In some embodiments, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 20% or less oxygen. In further embodiments, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 15% or less oxygen. In yet another embodiment, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 10% or less oxygen. In some embodiments, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 20% or less oxygen, about 15% or less oxygen, about 10% or less oxygen, or about 5% or less oxygen. In some embodiments, polymethylsilsesquioxane fine particles are heated in an atmosphere containing about 20%, about 15%, about 10%, about 5%, about 4%, about 3%, about 2%, or about 1% oxygen.

[0047] ii. Time In some embodiments, the polymethylsilsesquioxane particles are heated for about 10 minutes to about 1 hour. In further embodiments, the polymethylsilsesquioxane particles are heated for about 45 minutes. In some embodiments, the polymethylsilsesquioxane particles are heated for about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, or about 1 hour.

[0048] c.Characteristics In one embodiment, silica particles prepared by the method described herein have a median (D50) particle size ranging from about 0.5 μm to about 50 μm, as measured by laser diffraction.

[0049] i. Particle size In some embodiments, the silica particles have a median (D50) particle size ranging from about 0.5 μm to about 50 μm. In further embodiments, the silica particles have a median (D50) particle size ranging from about 1 μm to about 20 μm. In another embodiment, the silica particles have a median (D50) particle size ranging from about 1 μm to about 10 μm. In yet another embodiment, the silica particles have a median (D50) particle size ranging from about 1 μm to about 5 μm. In some aspects, silica particles have a median (D50) particle size of approximately 0.5, 0.75, 1, 1.25, 1.5, 1.75, 2, 2.25, 2.5, 2.75, 3, 3.25, 3.5, 3.75, 4, 4.25, 4.5, 4.75, 5, 10, 15, 20, 25, 30, 35, 40, 45, or 50 μm.

[0050] In some embodiments, the silica particles have a D90 / D10 particle size distribution of approximately 1.3 or less, as measured by laser diffraction. In some embodiments, the silica particles have a D90 / D10 particle size distribution of approximately 1.0, approximately 1.1, approximately 1.2, or approximately 1.3.

[0051] ii. Sphericity of particles In some embodiments, the silica particles are spherical with a sphericity of greater than 0.9. In some embodiments, the silica particles are spherical with a sphericity of between 0.9 and 1.

[0052] iii.Particle surface In some embodiments, silica particles are non-porous.

[0053] In some embodiments, the silica particles are surface-treated with at least one hydrophobic agent. In some embodiments, the hydrophobic agent is alkylsilane (e.g., triethoxycaprylylsilane or dimethylsilyl agents), metal soap (e.g., isopropyl titanium triisostearate), stearyl-modified amino acids (e.g., disodium stearoyl glutamate and aluminum hydroxide), silicone (e.g., dimethicone), fluoride (e.g., perfluorooctyltriethoxysilane), and mixtures thereof. In some embodiments, the hydrophobic agent is hexamethyldisilazane.

[0054] IV. Personal Care In a further aspect of this disclosure, the products of this disclosure, namely silica particles, may be incorporated into personal care items.

[0055] In some embodiments, personal care items may be cosmetics or medical products.

[0056] In one embodiment, the personal care composition further comprises preservatives, antioxidants, binders, defoamers, antistatic agents, colorants, emulsifying stabilizers, oxidizing agents, propellants, opacifiers, UV filters, UV absorbers, modifiers, viscosity modifiers, modifiers, chelating agents, gums or thickeners, oils, waxes, fragrances, essential oils, emulsifiers, surfactants, and combinations thereof.

[0057] In some embodiments, personal care compositions may be formulated with preservatives, antioxidants, chelating agents, gums or thickeners, oils, waxes, fragrances, essential oils, emulsifiers, surfactants, and combinations thereof.

[0058] In some embodiments, the products of the present disclosure may be added to formulations comprising makeup, color cosmetics, foundations, blushes, lipsticks, lip balms, eyeliners, mascaras, oil removers, color cosmetic removers, and powders.

[0059] In some embodiments, the products of the present disclosure are compounded with hydrophobic powders. Hydrophobic powders can be obtained by hydrophobizing the surface of one or more organic or inorganic powders. In some embodiments, one or more organic or inorganic powders may include, but are not limited to, silicone resin particles, nylon-12, PMMA, cellulose, modified starch, talc, boron nitride, polyurethane, and kaolin particles.

[0060] Personal care compositions may have personal care applications including deodorants, antiperspirants, antiperspirant / deodorants, shaving products, skin lotions, moisturizers, cosmetics, bath products, cleansing products, hair care products such as shampoos, conditioners, mousses, styling gels, hair sprays, hair dyes, hair color products, hair bleaches, wave products, hair straighteners, manicure products (e.g., nail polish, nail polish remover, nail creams and lotions, cuticle softeners), protective creams (e.g., sunscreens, insect repellents and anti-aging products), color cosmetics (e.g., lipsticks, foundations, face powders, eyeliners, eyeshadows, blushes, makeup, mascaras), and dental care (e.g., toothpaste). Personal care applications may also include drug delivery systems for topical application of pharmaceutical compositions that can be applied to the skin.

[0061] In one embodiment, the personal care composition further comprises one or more personal care ingredients. Suitable personal care ingredients include, but are not limited to, emollients, moisturizers, humectants, pigments (e.g., pearlescent pigments such as mica coated with bismuth oxychloride and titanium dioxide), colorants, fragrances, biocides, preservatives, antioxidants, antifungal agents, antiperspirants, exfoliants, hormones, enzymes, medicinal compounds, vitamins, salts, electrolytes, alcohols, polyols, UV absorbers, plant extracts, surfactants, silicone oils, organic oils, waxes, film-forming agents, thickeners (e.g., fumed silica or hydrated silica), and particulate fillers (e.g., talc, kaolin, starch, modified starch, mica, nylon, clay, e.g., bentonite and organically modified clay).

[0062] In some embodiments, one or more personal care ingredients included in the personal care composition are selected from the group consisting of humectants, emollients, moisturizers, pigments, colorants, fragrances, biocides, preservatives, antioxidants, antifungal agents, antiperspirants, exfoliants, hormones, enzymes, medicinal compounds, vitamins, salts, electrolytes, alcohols, polyols, UV absorbers, plant extracts, surfactants, silicone oils, organic oils, waxes, film-forming agents, and thickeners. In some embodiments, one or more emollients are selected from the group consisting of triglyceride esters, wax esters, alkyl or alkenyl esters of fatty acids, polyhydric alcohol esters, and mixtures thereof. In some embodiments, one or more personal care ingredients are silicone oils, organic oils, or mixtures thereof.

[0063] In one embodiment, the personal care composition is an antiperspirant composition comprising a polymer composition or product described herein and one or more active antiperspirants. Suitable antiperspirants include, but are not limited to, Category I active antiperspirant ingredients as described in the U.S. Food and Drug Administration's Monograph of October 10, 1993, relating to human antiperspirant products available without a prescription, such as aluminum halides, aluminum hydroxy halides, such as aluminum chlorohydrate, and complexes or mixtures thereof with zirconyl oxy halides and zirconyl hydroxy halides (e.g., aluminum-zirconium chlorohydrate and aluminum zirconium glycine complexes such as aluminum-zirconium tetrachlorohydrate glycine).

[0064] In another embodiment, the personal care composition is a skincare composition comprising the polymer composition or product described herein and a vehicle such as a silicone oil or organic oil. The skincare composition may also comprise emollients, such as triglyceride esters, wax esters, alkyl or alkenyl esters or polyhydric alcohol esters of fatty acids, pigments, vitamins (e.g., vitamin A, vitamin C, and vitamin E), sunscreen or sunblock compounds (e.g., titanium dioxide, zinc oxide, oxybenzone, octyl methoxycinnamate, butyl methoxydibenzoylmethane, p-aminobenzoic acid, and octyldimethyl-p-aminobenzoic acid).

[0065] In yet another embodiment, the personal care composition is a color cosmetic composition such as a lipstick, makeup, or mascara. The color cosmetic composition comprises a polymer composition or product as described herein, and a colorant (e.g., a pigment, a water-soluble dye, or a lipid-soluble dye). [Examples]

[0066] The following examples are included to demonstrate various aspects of this disclosure. Those skilled in the art should understand that the techniques disclosed in the following examples represent techniques that the inventors have found to function well in the implementation of this disclosure and can therefore be considered to constitute a preferred form for its implementation. However, those skilled in the art should understand that many modifications can be made to the specific examples disclosed in light of this disclosure, and that similar or comparable results can still be obtained without departing from the spirit and scope of the disclosure.

[0067] Example 1: Preparation of spherical particles (A) 500 g of polymethylsilsesquioxane microparticles (Momentive TOSPEARL 145A) with an average particle size of 4.5 μm were added to a suitable container with dimensions of 415 x 415 x 50 mm (width x depth x height), and the mixture was heated at 500°C for 30 minutes in an atmosphere of 10% oxygen in nitrogen-mixed air. Next, the particles were heated at 400°C for 45 minutes in an air atmosphere. 445 g of spherical silica microparticles (A) were obtained. The median (D50) particle size of the obtained spherical silica microparticles was 3.8 μm, the particle size distribution D90 / D10 was 1.11, and the BET specific surface area was 1.32 m² as measured by TriStar II Plus (Micromeritics, Norcross, Georgia). 2 It was / g.

[0068] Example 2: Preparation of spherical particles (B) In a suitable container with dimensions of 415 x 415 x 50 mm (width x depth x height), 500 g of polymethylsilsesquioxane microparticles (Momentive TOSPEARL 120A) with an average particle size of 2 μm was added and heated at 450°C for 5 hours in an air atmosphere. 448 g of spherical silica microparticles (B) were obtained. The median (D50) particle size of the obtained spherical silica microparticles was 1.7 μm, the particle size distribution D90 / D10 was 1.17, and the specific surface area was 2.7 m² as measured by TriStar II Plus. 2 It was / g.

[0069] Example 3: Preparation of spherical particles (C) In a suitable container with dimensions of 415 x 415 x 50 mm (width x depth x height), 300 g of polymethylsilsesquioxane microparticles (Momentive TOSPEARL 1110A) with an average particle size of 11 μm was added and heated at 500°C for 30 minutes in a nitrogen-mixed air atmosphere with an oxygen concentration of 10%. Next, the particles were heated at 400°C for 45 minutes in an air atmosphere. 267 g of spherical silica microparticles (C) were obtained. The median (D50) particle size of the obtained spherical silica microparticles was 9.4 μm, the particle size distribution D90 / D10 was 1.08, and the specific surface area was 0.6 m² as measured by TriStar II Plus. 2 It was / g.

[0070] Example 4: Preparation of surface-treated spherical particles (D) In a suitable container, 20 grams of spherical silica particles (A) were dispersed in 10 grams of water. The mixture was mixed using an overhead stirrer (IKA Eurostar 100 digital overhead stirrer). Next, 6 grams of hexamethyldisilazane were added to the mixture, and the mixture was stirred at 25°C for 6 hours. The slurry was then dried at 150°C for 3 hours. The dried powder was then sieved through a 50-micron sieve. The resulting spherical powder (D) had a median particle size (D50) of approximately 3.8 microns. The particle size distribution, measured as D90 / D10, was 1.11.

[0071] Example 5: Powder foundation Powder foundations were prepared using the above-mentioned silica microparticles (A) to (C), Tospearl microparticles, and silica microparticles, with the compositions shown in Table 1. In the preparation method, the raw materials for phases A and B were first mixed in a Hanil Lab mixer, then the pre-mixed raw materials for phase C were added, and the mixture was uniformly mixed again using the Hanil Lab mixer. Finally, the mixture was compressed and molded into a metal plate. [Table 1A] [Table 1B]

[0072] The evaluation results for "spreadability," "skin smoothness," "blendability," "soft-focus effect," and "makeup longevity after 12 hours" are also shown in Table 2 along with the composition. The evaluation was conducted by 10 panelists who scored each item according to the following criteria, and the average score was used for the final evaluation.

[0073] "Excellent": 5 points; "Good": 4 points; "Average": 3 points; "Poor": 2 points; and "Poor": 1 point. [Table 2]

[0074] Example 6; Powder formulation The powder formulation was prepared using the silica microparticles (A) described in Example 1 and comparative spherical silica (Sunsphere NP-30, AGC SI-TEC Co., Ltd.) having an average particle size of 4 microns and a D90 / D10 ratio of 2.7, with the composition shown in Table 3 below. The raw materials were mixed in a 100 gm speed mixer container, and the powder was mixed for 5 minutes to obtain a uniformly mixed, loose powder formulation.

[0075] The coefficient of friction of the powder formulation was measured using a CSM Tribometer. The powder was then lasered (2 mg / cm³). 2 The material was rubbed against the surface for 10 seconds. Friction was measured using a 1 cm diameter stainless steel probe on a flat surface of leather (Testfabrics Inc.). Friction was measured at a speed of 1 cm / second for a probe that reciprocated 10 cycles around 2 cm. The coefficient of friction was reported as the average coefficient of friction over 10 cycles. [Table 3]

[0076] Figure 1 shows that a powder formulation with silica having a narrow particle size distribution (D90 / D10=1.1) exhibited a lower coefficient of friction than a formulation with a wider particle size distribution (D90 / D10=2.7). Figures 3A and 3B show the particle size distribution of spherical particles for Example 1 (D90 / D10=1.1, D50=3.9μm) and comparative silica (D90 / D10=2.70, D50=4.3μm).

[0077] Example 7: Emulsified foundation Using the silica microparticles (A) described above, an emulsified foundation with the following composition was prepared. The preparation method involved first mixing raw materials (5) to (8) in a Henschel mixer, then adding raw materials (1) and (3) to (4), thoroughly mixing the mixture, and then grinding and separating it. Further, raw materials (2) and (9) to (18) were added, the mixture was treated in a homomixer, degassed, and then filled into containers. [Table 4]

[0078] Example 8: Powder foundation Using the above-mentioned silica fine particles (A), a powder foundation serving two purposes with the following composition was prepared. The preparation method involved first mixing raw materials (1) and (3) through (10), grinding them, transferring them to a Henschel mixer, and then adding raw materials (2) and (11) through (16) and mixing them uniformly. Next, the mixture was compressed and molded into a metal plate. [Table 5]

[0079] Example 9: Powdered eyeshadow Using the above-mentioned silicone particles (A), a powder eyeshadow with the following composition was prepared. The preparation method involved first mixing raw materials (1) and (3) through (10) and grinding them, then transferring them to a Henschel mixer, then adding raw materials (2) and (11) and mixing them uniformly, and finally compressing the mixture into a metal plate. [Table 6]

[0080] Example 10: Two-layer separation sunscreen Using the above-mentioned silicone particles (A), a two-layer separation type sunscreen emulsion having the following composition was prepared. In the preparation method, raw materials (1) to (7) were first dispersed and mixed using a disperser, and then aqueous phase raw materials (8) to (11) were added and stirred to emulsify. [Table 7]

[0081] Example 11. Sunscreen cream Using the above-mentioned silicone particles (A), a sunscreen cream with the following composition was prepared. In the preparation method, raw materials (1) to (8) were first dispersed and mixed using a disperser, and then aqueous phase raw materials (8) to (10) were added and stirred to emulsify. [Table 8]

[0082] Example 12: Solid white powder Using the silicone particles (A) described above, a solid white powder with the following composition was prepared. The preparation method involved first mixing raw materials (1) and (3) through (6), grinding them, transferring them to a Henschel mixer, then adding raw materials (2) and (7) through (10) and mixing them uniformly, and finally compressing the mixture into a metal plate. [Table 9]

[0083] Example 13: Blush Using the above-mentioned silica microparticles (A), a blush having the following composition was prepared. The preparation method involved first mixing and crushing raw materials (1) to (6), transferring them to a Henschel mixer, adding raw materials (7) to (10) and mixing them uniformly, and then compressing and molding them into a metal plate. [Table 10]

[0084] Example 14: Lipstick Using the above-mentioned silica nanoparticles (A), a lipstick with the following composition was prepared. The preparation method involved heating and dissolving raw materials (1) to (11), then adding and mixing (12) and (13), degassing the mixture, pouring it into a container, and rapidly cooling it to harden it. [Table 11]

[0085] Example 15: Skin Primer Using the above-mentioned silica nanoparticles (A), a skin primer with the following composition was prepared. The preparation method involved heating and mixing raw materials (1) to (7), thoroughly mixing raw materials (8) to (13) separately, then adding them to raw materials (1) to (7) and mixing thoroughly, and finally adding aqueous phase raw materials (14) to (18) and stirring to emulsify. [Table 12]

[0086] Example 16: BB cream Using the silica microparticles (A) described above, a BB cream with the following composition was prepared. The preparation method involved mixing raw materials (1) to (9) until uniform, thoroughly mixing raw materials (10) to (15) separately, then adding them to raw materials (1) to (9) and mixing well, then adding aqueous phase raw materials (16) to (21) and mixing well, and finally adding (22) to homogenize and make the mixture uniform. [Table 13]

[0087] Example 17: CC cream Using the silica microparticles (A) described above, a CC cream with the following composition was prepared. The preparation method involved mixing raw materials (5) to (14) until homogeneous, thoroughly mixing raw materials (15) to (17) separately, then adding them to raw materials (5) to (14) and mixing well, then adding aqueous phase raw materials (1) to (4) and mixing well, and finally adding (18) to (20) and mixing until homogeneous. [Table 14]

[0088] Example 18: Mascara Using the silica microparticles (A) described above, a mascara with the following composition was prepared. The preparation method involved mixing raw materials (3) and (4) with water and heating to make them homogenized, adding raw materials (2) and (5) to (9) and mixing well, heating raw materials (10) to (15) separately, then adding them to the mixture and mixing well, then cooling to 45°C, and adding raw materials (16) and (17) one by one and mixing to make them homogenized. [Table 15]

[0089] Example 19: Concealer Using the silica microparticles (A) described above, a concealer with the following composition was prepared. The preparation method involved mixing raw materials (1) and (7) until homogeneous, heating to 90°C, adding raw materials (8) through (10), mixing until homogeneous, and pouring the mixture into a suitable container. [Table 16]

[0090] Example 20; O / W cream Using the silica microparticles (A) described above, an O / W cream with the following composition was prepared. The preparation method involved mixing raw materials (1) to (3) and heating to 80°C, separately mixing raw materials (4) to (6) and adding them to raw materials (1) to (3), mixing until homogeneous, cooling to room temperature, and then adding raw materials (7) and (8) and mixing until homogeneous. [Table 17]

[0091] Example 21: W / O cream Using the silica microparticles (A) described above, a W / O cream with the following composition was prepared. The preparation method involved mixing raw materials (1) to (6) and heating to 70°C, separately mixing raw materials (7) to (9) and adding them to raw materials (1) to (6), mixing to emulsify, and then cooling to room temperature. [Table 18]

[0092] Example 22: Eye cream Using the silica microparticles (A) described above, an eye cream with the following composition was prepared. The preparation method involved mixing raw materials (1) to (4) and heating to 70°C, separately mixing raw materials (5) to (12) and heating to 70°C, then adding them to raw materials (1) to (4), mixing and emulsifying, then cooling to 50°C, adding raw material (13), and mixing until homogeneous. [Table 19]

[0093] Example 23: Skin serum Using the surface-treated silica microparticles (D) described above, a skin serum with the following composition was prepared. The preparation method involved mixing raw materials (1) to (4) until homogeneous, mixing raw materials (5) to (7) separately, adding them to raw materials (1) to (4) and mixing until homogeneous, then adding raw materials (8) to (11) one by one and mixing until homogeneous. [Table 20]

[0094] Example 24: Shampoo Using the silica microparticles (A) described above, a shampoo with the following composition was prepared. The preparation method involved adding raw material (3) to water, mixing it uniformly, heating it to 80°C, and after the mixture became transparent, adding raw materials (2) and (5) through (10) one by one, confirming that the mixture remained transparent, cooling it to room temperature, and then adding raw materials (11) through (15) one by one, mixing until uniform. [Table 21]

[0095] It should be understood that the section describing embodiments for carrying out the invention, rather than the section describing the summary and abstract of the invention, is intended to be used to interpret the claims. The section describing the summary and abstract of the invention may describe one or more exemplary embodiments, though not all, of the disclosure contemplated by the inventor, and is therefore not intended to limit the scope of the disclosure and the accompanying claims in any way.

[0096] This disclosure has been described above with the help of functional foundational elements that describe the implementation of specific functions and their relationships. The boundaries of these functional foundational elements are arbitrarily defined herein for the sake of clarity. Alternative boundaries can be defined as long as the specific functions and their relationships are adequately implemented.

[0097] The foregoing descriptions of specific embodiments fully reveal the general nature of the disclosure so that others, by applying knowledge within the scope of the art, can readily modify and / or adapt them for various uses, such as those specific embodiments, without diverting from the general concepts of the disclosure and without excessive experimentation. Such adaptations and modifications are therefore intended to fall within the equivalent meaning and scope of the disclosed embodiments based on the teachings and guidance presented herein. It should be understood that the words and terms herein are for illustrative purposes only and not limiting, and that they are to be interpreted by those skilled in the art in light of the teachings and guidance.

[0098] The scope and breadth of this disclosure should not be limited by any of the exemplary embodiments described above, but should be defined solely in accordance with the following claims and their equivalents.

[0099] Other embodiments All publications, patents, and patent applications referenced herein are incorporated herein by reference in the same manner as any individual publication, patent, or patent application is specifically and individually indicated to be incorporated herein by reference in whole. Where a term used in this application is found to be defined differently in any document incorporated herein by reference, the definition provided herein shall serve as the definition of that term.

[0100] While this disclosure has been described in relation to its particular aspects, it will be understood that this disclosure is subject to further modification, and this application is intended to cover any modifications, uses, or adaptations of the invention, including any deviations from this disclosure in accordance with the claimed scope, and which are applicable to the essential features described above, and which are generally in accordance with the principles of the invention and which are within the scope of known or practice in the art to which the invention pertains.

Claims

1. (SiO ４／２ Silica particles containing repeating units of ), wherein the silica particles are obtained by heating polymethylsilsesquioxane fine particles in an atmosphere containing 5% to 15% oxygen at a temperature of 500°C or less, and the silica particles have a D90 / D10 particle size distribution of 1.3 or less as measured by a particle size analyzer using laser diffraction particle size analysis, wherein the silica particles are spherical and have a sphericity of 0.9 or more as defined by the short axis / long axis, and 0.1 m ２ / g to 5m ２ Silica particles with a BET surface area of ​​1 / g, useful for personal care formulations.

2. The silica particles according to claim 1, wherein the silica particles have a D90 / D10 particle size distribution of 1.0 to 1.

2.

3. The silica particles according to claim 1, wherein the silica particles have a median (D50) particle size of 0.5 μm to 50 μm.

4. The silica particles according to claim 1, wherein the silica particles have a sphericity of 0.95 or more, defined by the short axis / long axis.

5. The silica particles according to claim 1, wherein the silica particles are non-porous.

6. The silica particles according to claim 1, wherein the silica particles are surface-treated with at least one hydrophobic agent.

7. The silica particles according to claim 6, wherein the hydrophobic agent is selected from the group consisting of alkylsilanes, metal soaps, stearyl-modified amino acids, silicones, fluorinated silanes, natural esters, and combinations thereof.

8. The silica particles according to claim 6, wherein the hydrophobic agent is hexamethyldisilazane.

9. (SiO ４／２ A method for producing silica particles containing repeating units of ), the method comprising heating polymethylsilsesquioxane fine particles in an atmosphere containing 5% to 15% oxygen at a temperature of 500°C or less to form silica particles, wherein the silica particles have a D90 / D10 particle size distribution of 1.3 or less as measured by a particle size analyzer utilizing laser diffraction particle size analysis, are spherical, and have a sphericity of 0.9 or more as defined by the short axis / long axis, and 0.1 m ２ / g to 5m ２ A method useful for personal care formulations having a BET surface area of ​​1 / g.

10. The method according to claim 9, wherein the polymethylsilsesquioxane fine particles are heated for 10 minutes to 6 hours.

11. The method according to claim 9, further comprising lowering the temperature to 400°C.

12. The method according to claim 9, wherein the polymethylsilsesquioxane fine particles are heated for 10 minutes to 1 hour.

13. The method according to claim 9, wherein the polymethylsilsesquioxane fine particles are heated in an electric furnace, a gas furnace, a far-infrared furnace, a mid-infrared furnace, or a near-infrared furnace.

14. Silica particles prepared by the method of claim 9, wherein the silica particles have a median (D50) particle size of 0.5 μm to 50 μm as measured by laser diffraction.

15. Silica particles having an average particle size of 0.5 μm to 20 μm, prepared by the method of claim 9.

16. Silica particles prepared by the method of claim 9, wherein the silica particles are spherical, having a sphericity greater than 0.9 as defined by the short axis / long axis.

17. Silica particles prepared by the method of claim 9, wherein the silica particles are non-porous.

18. A personal care formulation containing silica particles as described in claim 1.

19. The personal care formulation according to claim 18, further comprising preservatives, antioxidants, binders, defoamers, antistatic agents, colorants, emulsifying stabilizers, oxidizing agents, propellants, opacifiers, UV filters, UV absorbers, denaturants, viscosity modifiers, chelating agents, gums or thickeners, oils, waxes, fragrances, essential oils, emulsifiers, surfactants, and combinations thereof.

20. The personal care formulation according to claim 19 is a deodorant, antiperspirant, skin cream, facial cream, hair shampoo, hair conditioner, mousse, hair styling gel, hair spray, protective cream, lipstick, lip color, facial foundation, blush, makeup, and mascara, skincare lotion, moisturizer, facial treatment, personal cleanser, facial cleanser, bath oil, perfume, shaving cream, pre-shave lotion, after-shave lotion, cologne, sachet, toothpaste, or sunscreen.

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