WO2024106708A1 - Microcapsule containing high content of oil and amorphous silica, and method for producing same - Google Patents

Microcapsule containing high content of oil and amorphous silica, and method for producing same Download PDF

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Publication number
WO2024106708A1
WO2024106708A1 PCT/KR2023/013408 KR2023013408W WO2024106708A1 WO 2024106708 A1 WO2024106708 A1 WO 2024106708A1 KR 2023013408 W KR2023013408 W KR 2023013408W WO 2024106708 A1 WO2024106708 A1 WO 2024106708A1
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Prior art keywords
microcapsule
oil
inorganic powder
microcapsules
amorphous silica
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PCT/KR2023/013408
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French (fr)
Korean (ko)
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고태성
이진홍
홍민표
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(주)바이오제닉스
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11—Encapsulated compositions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin

Definitions

  • the present invention relates to microcapsules containing a high content of oil and amorphous silica and a method for producing the same, and more specifically, to a microcapsule that can be produced by a physical method without additives and a method for producing the same.
  • Microcapsules are composed of a core and a shell surrounding the core, and have the characteristic of protecting the core material containing an unstable or weakly lasting active ingredient through the shell and releasing it at an appropriate time. Microcapsules can be used in a variety of fields depending on the type of core material. They are especially useful in the cosmetics field because they are easy to handle and can easily mix substances that do not mix well, such as oil and water.
  • microcapsules that use polymers or wax as shells have a difficult problem when applied to cosmetic formulations. Since the maturation characteristics of the shell also change as the formulation of the cosmetic changes, it is difficult to universally apply it to cosmetics of various formulations, and the stability of the microcapsules may be reduced due to the maturation characteristics.
  • microcapsules were manufactured by chemical methods such as sol-gel process and interfacial polymerization.
  • additives such as catalysts, surface treatment agents, and surfactants are required.
  • the manufacturing process of microcapsules becomes complicated, and it is difficult to remove the additives from the microcapsules, so the manufactured microcapsules may contain the additives.
  • a cosmetic composition containing microcapsules containing additives is applied to the skin, it may cause skin diseases such as rashes and hives, which may lead to safety issues.
  • Korean Patent Publication No. 10-2015-0082870 manufactured a Pickering emulsion using powdered polymethylmethacrylate and silica powder instead of an emulsifier.
  • Pickering emulsion is difficult to maintain the stability of the interface between the water phase and the oil phase, and is vulnerable to external environmental changes such as acids, bases, and temperature, so there is a risk that the emulsion is easily destroyed.
  • microcapsules that do not contain additives and do not have a negative effect on the skin, have a simple manufacturing method, and are not affected by the formulation of the cosmetic, so they can be widely applied to various types of cosmetics. .
  • the purpose of the present invention is to solve the problems of the prior art, and to provide microcapsules that contain a high content of oil and do not require additives such as catalysts, surface treatment agents, and surfactants during production, and a method for producing the same. .
  • the microcapsule according to the present invention is a microcapsule comprising a core containing oil and inorganic powder and a shell in which a plurality of amorphous silica particles are densely assembled located on the core, and is 80 to 80% based on the total weight of the microcapsule. It contains 99% by weight of oil and inorganic powder, and the shell is characterized by being porous.
  • the amorphous silica particles may contain 1 to 20% by weight based on the total weight of the microcapsule.
  • the weight of the inorganic powder may be greater than the oil.
  • the weight ratio of oil and inorganic powder contained in the microcapsules may be 1:1.5 to 1:4.
  • the average particle diameter (D 50 ) of the amorphous silica particles may be 400 to 500 nm.
  • the particle size distribution width ((D 90 -D 10 )/D 50 ) of the amorphous silica particles may be 0.9 to 1.2.
  • the shell may be a porous shell including pores with a particle diameter of 200 to 800 nm.
  • the average particle diameter of the microcapsules may be 30 to 300 ⁇ m.
  • the inorganic powder may include a hydrophilic inorganic powder complexed with a fatty acid salt.
  • the inorganic powder may include a hydrophobic inorganic powder complexed with polyol.
  • the inorganic powder is titanium dioxide, iron oxide pigment, organic pigment, lake dye, natural pigment, synthetic fluorophlogopite, zinc oxide, boron nitride, talc, kaolin, mica, sericite, barium sulfate, and sheet alumina. , pearl, or mixtures thereof.
  • the cosmetic composition according to the present invention may contain the above microcapsules.
  • the present invention includes the method for producing the above-described microcapsules.
  • the method for producing microcapsules according to the present invention includes preparing a dispersion containing amorphous silica particles, oil, inorganic powder, and solvent; and spray-drying the dispersion using a rotary spray dryer to produce microcapsule particles, wherein the oil and inorganic powder contain 10 to 30% by weight based on the total weight of the dispersion.
  • the step of sorting the microcapsule particles by passing them through a sieve classifier may be further included.
  • the solvent may include one selected from the group including ethanol and acetone.
  • microcapsule according to the present invention is not limited by the formulation of the cosmetic and can be applied to various formulations.
  • microcapsules do not contain additives, they may not cause skin irritation.
  • the present invention provides a microcapsule that contains a high content of oil and can provide a unique feeling of use and excellent moisturizing power to the user when applied to a water-based cosmetic, and a method of manufacturing the same.
  • Figure 1 is a photograph of the surface of a microcapsule (a) manufactured by the method according to Example 2 and a microcapsule (b) manufactured by the method according to Example 3 observed with a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • Figure 2 is a photograph of the surface of a microcapsule manufactured by the method according to Comparative Example 1 observed with a scanning electron microscope (SEM).
  • Figure 3 is a photograph of the surface of a microcapsule manufactured by the method according to Example 7 observed with a scanning electron microscope (SEM).
  • Figure 4 is a photograph of the surface of a microcapsule (a) manufactured by the method according to Example 9 and a microcapsule (b) manufactured by the method according to Example 10 observed with a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • microcapsule containing amorphous silica of the present invention and its manufacturing method will be described in detail.
  • the terms used in this specification are general terms that are currently widely used as much as possible while considering the function of the present invention, but this may vary depending on the intention or precedent of a technician working in the related field, the emergence of new technology, etc. Unless otherwise defined, the technical and scientific terms used may have meanings commonly understood by those skilled in the art in the technical field to which this invention belongs.
  • the numerical range used in this specification includes the lower limit and upper limit and all values within the range, increments logically derived from the shape and width of the defined range, all double-defined values, and the upper limit of the numerical range defined in different forms. and all possible combinations of the lower bounds. Unless otherwise specified in the specification of the present invention, values outside the numerical range that may occur due to experimental error or rounding of values are also included in the defined numerical range.
  • the microcapsule according to the present invention includes a core containing oil and inorganic powder and a shell in which a plurality of amorphous silica particles are densely assembled located on the core, and contains 80 to 99% by weight of the total weight of the microcapsule. of oil and inorganic powder, and the shell is porous.
  • Microcapsules with a core-shell structure which includes a core containing oil and inorganic powder and a shell surrounding the core and densely assembled with a plurality of amorphous silica particles, can have excellent stability without any additional additives and can be used in various formulations. It can be widely applied to cosmetics. In addition, it has the advantage of being able to contain a high content of oil and inorganic powder contained in the core due to its high specific surface area.
  • organic materials such as organic polymers or wax are mainly used as the shell of microcapsules used in cosmetics.
  • microcapsules containing organic substances as shells to cosmetics, there is a problem in that the maturation conditions are difficult because the maturation characteristics of the microcapsules vary depending on the formulation of the cosmetic. Even if the ripening characteristics of the microcapsules are not suitable for the formulation of the cosmetic, the usability and stability of the cosmetic containing the microcapsules may be extremely reduced.
  • amorphous silica which is an inorganic material
  • the aging characteristics of amorphous silica may not be affected even if the formulation of the cosmetic is changed, and more advantageously, the aging process may not be necessary.
  • the shell of the microcapsule contains amorphous silica, it is advantageous in terms of versatility because it can have excellent feeling of use and excellent stability in various formulations regardless of the formulation of the cosmetic.
  • the shell of the microcapsule may be a dense assembly of a plurality of amorphous silica particles, and the average particle diameter (D 50 ) of the amorphous silica particles forming the shell may be 400 to 500 nm or 420 to 480 nm, preferably may be 440 to 460 nm. Alternatively, it may be 400 nm or more, 410 nm or more, 420 nm or more, 430 nm or more, or 440 nm or more, and the upper limit may be 500 nm or less, 490 nm or less, 480 nm or less, 470 nm or less, 460 nm or less, or 450 nm or less.
  • Amorphous silica having an average particle size in the above range has a particle size that is significantly smaller than that of the microcapsule, so the amorphous silica can be densely assembled in the shell of the microcapsule.
  • the particle size distribution width ((D 90 -D 10 )/D 50 ) of the amorphous silica particles may be 0.90 to 1.20, 0.94 to 1.16, or 0.98 to 1.12, and preferably 1.0 to 1.10 days. You can. Or it may be 0.90 or more, 0.92 or more, 0.94 or more, 0.96 or more, 0.98 or more, or 1.0 or more, and the upper limit may be 1.2 or less, 1.18 or less, 1.16 or less, 1.14 or less, 1.12 or less, or 1.10 or less.
  • the particle size distribution width can be expressed in Equation 1 below.
  • Particle size distribution width (D 90 -D 10 )/D 50
  • D 90 , D 50 , and D 10 refer to the particle size of amorphous silica when the cumulative percentage reaches 90%, 50%, and 10%, respectively, in the particle size distribution of the entire amorphous silica.
  • a narrower particle size distribution means that amorphous silica can have a monodisperse particle size distribution with a smaller particle size deviation.
  • a plurality of amorphous silica particles contained in the shell have a narrow particle size distribution width and can have a uniform particle size. It is advantageous because uniform nano-sized amorphous silica particles are densely assembled in the shell of the microcapsule, making it possible to manufacture microcapsules with higher sphericity. Microcapsules with high sphericity can have a smooth surface without a rough surface texture, so when applied to the skin, there is less foreign body sensation and can provide an excellent feeling of use.
  • the shell may have porosity due to empty spaces between a plurality of amorphous silica particles.
  • the average particle diameter of the pores included in the shell may be 200 to 800 nm, 250 to 750 nm, 300 to 700 nm, 350 to 650 nm, or 400 to 600 nm.
  • it may be 200 nm or more, 250 nm or more, 300 nm or more, 350 nm or more, or 400 nm or more
  • the upper limit may be 800 nm or less, 750 nm or less, 700 nm or less, 650 nm or less, or 600 nm or less.
  • the shell of the microcapsule may include pores having the above particle size range to improve the surface area. As the surface area of the shell increases, the core of the microcapsule can contain a larger amount of oil. Additionally, when releasing oil to the outside of the microcapsule, the porous shell can be easily destroyed by simply applying a small impact to the microcapsule using a brush or hand, allowing the core material to be easily released.
  • the microcapsules can have excellent surface area. Therefore, it is advantageous because amorphous silica can absorb a large amount of oil and support a larger amount of oil in the core of the microcapsule.
  • the BET surface area of amorphous silica may be 100 to 200 m 2 /g, 110 to 190 m 2 /g, or 120 to 180 m 2 /g, and may be substantially 125 to 175 m 2 /g.
  • it may be 100 m 2 /g or more, 105 m 2 /g or more, 110 m 2 /g or more, 115 m 2 /g or more, 120 m 2 /g or more, or 125 m 2 /g or more, with the upper limit being 200 m 2 /g or less, 195 m 2 /g or less, 190 m 2 /g or less, 185 m 2 /g or less, or 180 m 2 /g or less, or 175 m 2 /g or less.
  • the amorphous silica may comprise 1 to 20%, 3 to 18%, 5 to 16%, 7 to 14% and 9 to 12% by weight relative to the total weight of the microcapsule. . Since the microcapsule contains amorphous silica with a large surface area in the above weight ratio, the weight of the amorphous silica is significantly less than that of the core material, but it can effectively surround the core material, making it possible to easily manufacture spherical microcapsules.
  • the stability of the microcapsule may be reduced due to insufficient envelopment of the core material, and if it contains amorphous silica of more weight% than the above range, the viscosity increases. As a result, there is a risk that microcapsules with low sphericity may be produced and the feeling of use may be reduced.
  • the oil and inorganic powder which are the core materials of the microcapsule, are 80 to 99% by weight, 82 to 97% by weight, 84 to 95% by weight, 84 to 93% by weight, and 85 to 85% by weight, based on the total weight of the microcapsule. It may contain 90% by weight.
  • the amorphous silica contained in the shell of the microcapsule not only has a large surface area but also has good oil absorption, so a large amount of oil can be contained in the core of the microcapsule compared to the weight of the shell.
  • the weight of the inorganic powder may be greater than that of the oil.
  • the weight ratio of oil and inorganic powder contained in the microcapsule may be 1:1.5 to 4, 1:1.6 to 3.8, 1:1.7 to 3.5, and 1:1.8 to 3.2, and preferably 1:1.8 to 3.0. .
  • microcapsules with a core-shell structure can contain more inorganic powder by weight than oil, which can improve performance when applied to cosmetic compositions.
  • the inorganic powder contains a color pigment in the above weight ratio, vivid color development can be achieved without lowering saturation during color development.
  • the inorganic powder includes functional powder, it can have excellent covering power, spreadability, and ultraviolet ray blocking effects.
  • the average particle diameter of the microcapsule may be 30 to 300 ⁇ m, 60 to 250 ⁇ m, 90 to 200 ⁇ m, or 100 to 180 ⁇ m. Alternatively, it may be 30 ⁇ m or more, 50 ⁇ m or more, 70 ⁇ m or more, 90 ⁇ m or more, or 100 ⁇ m or more, and the upper limit may be 300 ⁇ m or less, 250 ⁇ m or less, 230 ⁇ m or less, 200 ⁇ m or less, or 180 ⁇ m or less.
  • the present invention is not limited by the average particle size of the microcapsules, it is advantageous because it provides an excellent feeling of use due to less heterogeneity when applying microcapsules having the above particle size range to the skin.
  • fatty acid salts may be further included as an additive so that the microcapsules may contain the inorganic powder complexed with the fatty acid salts.
  • Hydrophilic inorganic powder which is the core material of microcapsules, and oil do not mix with each other, which can form an unstable state.
  • the unstable interface between inorganic powder and oil can be stabilized by adding fatty acid salts to microcapsules.
  • fatty acid salts may act as a water-insoluble thickener to increase the viscosity of cosmetics and improve adhesion.
  • the fatty acid salt may include one or more selected from the group including polyhydroxystearic acid, magnesium stearate, aluminum stearate, calcium laurate, calcium myristate, and magnesium palmitate.
  • polyol when the surface of the inorganic powder is hydrophobic, polyol may be further included as an additive, so that the microcapsules may include the hydrophobic inorganic powder complexed with the polyol.
  • Polyol contains hydroxyl groups, so it can dissolve solid components that are not easily soluble in water.
  • microcapsules containing hydrophobic inorganic powder complexed with polyol are added to the water formulation, the microcapsules are broken and the hydrophobic inorganic powder can be mixed with the water formulation without any discomfort due to the polyol. Therefore, it can provide the effect of improving the applicability and spreadability of cosmetics.
  • the polyol may include one or more selected from the group including dipropylene glycol, 1,3-butanediol, ethylene glycol, polyethylene glycol, diethylene glycol, glycerin, pentylene glycol, sorbitol, propanediol, and propylene glycol.
  • the amorphous silica may include hydrophilic or hydrophobic silica depending on the type of cosmetic composition.
  • the oil may include one or more selected from the group including hydrocarbon-based oil, ester-based oil, and natural oil.
  • the hydrocarbon-based oil may include one or more selected from the group including polybutene, hydrogenated polyisobutene, and hydrogenated polydecene.
  • Ester oils include cetyl ethyl hexanoate, isocetyl ethyl hexanoate, isocetyl myristate, isopropyl myristate, neopentyl glycol dicaprate, hexyl laurate, triethylhexanoin, ethylhexyl palmitate, and It may include one or more selected from the group containing isononyl isononanoate.
  • Natural oils include jojoba oil, sunflower seed oil, avocado oil, macadamia seed oil, MCT oil, olive oil, green tea seed oil, coconut oil, citron oil, rosehip oil, argan oil, camellia oil, hemp seed oil, evening primrose oil and apricot oil. It may include one or more vegetable oils selected from the group containing oils, or one or more mineral oils selected from the group containing liquid paraffin, petrolatum, and silicone oil.
  • Inorganic powders may include functional powders that improve the feeling of use of cosmetics and color pigments that provide color.
  • the functional powder may include one or more selected from the group including synthetic fluorophlogopite, zinc oxide, boron nitride, talc, kaolin, mica, sericite, barium sulfate, sheet alumina, and pearl.
  • the color pigment may include one or more selected from the group including titanium dioxide, iron oxide pigment, organic pigment, lake dye, and natural pigment, but the present invention is not limited by the specific type of the core material of the microcapsule.
  • the cosmetic composition according to the present invention may contain the above-described microcapsules.
  • microcapsules are advantageous because they are not limited to the formulation of cosmetics and can be widely applied to various formulations of cosmetics.
  • the shell has a large surface area, making it possible to form microcapsules containing a high content of oil, including amorphous silica, which can support a large amount of oil.
  • Water-based cosmetics containing microcapsules containing a high content of oil can have excellent moisturizing power and can improve adhesion and spreadability by containing various inorganic powders in the core of the microcapsules.
  • cosmetic compositions include softening lotion, astringent lotion, nourishing lotion, nourishing cream, massage cream, essence, eye cream, eye essence, cleansing cream, cleansing foam, cleansing water, pack, powder, body lotion, body cream, and body oil. And it can be applied to one skin care cosmetic selected from the group containing sunscreen. Alternatively, it can be applied to one color cosmetic selected from the group including makeup base, foundation, lipstick, lip gloss, face powder, two-way cake, eye shadow, and blusher, but the present invention is not limited by the specific type of cosmetic. no.
  • the material, structure, shape, size, etc. of the core and shell are the same or similar to the microcapsules described above, so the manufacturing method of microcapsules according to the present invention is described in detail in the microcapsules previously. Includes all contents.
  • the method for producing microcapsules according to the present invention includes preparing a dispersion containing amorphous silica particles, oil, inorganic powder, and solvent; and preparing microcapsule particles by spray drying the dispersion using a rotary spray dryer, wherein the oil and inorganic powder may contain 10 to 30% by weight based on the total weight of the dispersion.
  • microcapsules When manufacturing microcapsules using amorphous silica as a wall material, encapsulation was conventionally performed by chemical methods such as the sol-gel method or monomer synthesis. When manufacturing microcapsules by chemical methods, a large amount of additives such as catalysts, surface treatment agents, and surfactants are required. When additives are used, the manufacturing process of microcapsules becomes complicated, and a large amount of waste water may be discharged during the process of removing the additives. Additionally, since additives are not easily removed from microcapsules, additives may remain in the manufactured microcapsules. When microcapsules containing residual additives are applied to the skin, there is a risk that the additives may cause skin irritation and cause skin diseases such as rashes and hives.
  • microcapsules using the manufacturing method according to the present invention, it is easy to control the physical properties of the final product by manufacturing the microcapsules by a physical method, and a large amount of oil can be produced through a simple manufacturing process without using additives in the manufacturing process. Microcapsules containing it can be manufactured.
  • the solvent is a polar solvent and may include one selected from ethanol and acetone.
  • the solvent can be dried quickly within a short time in the spray drying step described later.
  • the solvent By shortening the exposure time of heat-sensitive microcapsules to high temperatures, microcapsules with high sphericity can be manufactured.
  • the oil and inorganic powder may contain 10 to 30% by weight, 12 to 29% by weight, 14 to 28% by weight, 16 to 27% by weight, or 18 to 26% by weight based on the total weight of the dispersion. . Or it may contain 10% by weight or more, 12% by weight or more, 14% by weight or more, 16% by weight or more, 18% by weight or more, 20% by weight or more, 22% by weight or more, or 24% by weight or more, with an upper limit of 30% by weight. It may contain oil and inorganic powder in an amount of less than 29% by weight, less than 28% by weight, less than 27% by weight, less than 26% by weight, or less than 25% by weight. By adding oil and inorganic powder in a weight ratio within the above range, the core of the manufactured microcapsule can contain a high content of oil and inorganic powder.
  • Microcapsules can be prepared by drying the prepared dispersion in a rotary spray dryer to remove the solvent in the dispersion.
  • the feed temperature to the rotary spray dryer may be 1 to 50°C, 3 to 40°C, 5 to 30°C, 10 to 25°C, or 10 to 20°C above the boiling point of the solvent.
  • microcapsules can be manufactured by evaporating the solvent contained in the dispersion in a short time.
  • the microcapsules are manufactured through a simple process of drying a dispersion of oil, amorphous silica, and inorganic powder in a solvent with a spray dryer, thereby reducing the amount of additives used, including surfactants, and wastewater. emissions can be effectively reduced. Therefore, it is advantageous to reduce costs and provide an environmentally friendly process.
  • the method may further include passing the microcapsules prepared through the spray drying step through a sieve classifier to select microcapsule particles.
  • Microcapsules having a particle size of 500 ⁇ m or less, 450 ⁇ m or less, 400 ⁇ m or less, 350 ⁇ m or less, or 300 ⁇ m or less can be selected through a sieve classifier.
  • the feeling of use can be improved without any feeling of incompatibility with the formulation.
  • microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of hydrophilic color pigment as inorganic powder, and 30 g of hydrogenated polydecene as oil were added.
  • microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophilic amorphous silica, 60 g of hydrophilic color pigment as inorganic powder, and 30 g of hydrogenated polydecene as oil were added.
  • microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of hydrophilic color pigment as inorganic powder, and 30 g of isononyl isononanoate as oil were added.
  • microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of hydrophilic color pigment as inorganic powder, 15 g of oil-hydrogenated polydecene, and 15 g of isononyl isononanoate were added. was manufactured.
  • microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 35 g of hydrophilic color pigment as inorganic powder, 25 g of synthetic fluorophlogopite, and 30 g of oil-hydrogenated polydecene were added. did.
  • microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of hydrophobic color pigment as inorganic powder, and 30 g of hydrogenated polydecene as oil were added.
  • microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 55 g of hydrophobic color pigment as an inorganic powder, 30 g of oil-hydrogenated polydecene, and 5 g of dipropylene glycol, a polyol, were added as an additive. was manufactured.
  • microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of synthetic fluorophlogopite, which is a functional powder as an inorganic powder, and 30 g of hydrogenated polydecene as an oil were added.
  • microcapsules were prepared in the same manner as in Example 1, except that 1 g of hydrophobic amorphous silica, 70 g of hydrophilic color pigment as inorganic powder, and 30 g of hydrogenated polydecene as oil were added.
  • amorphous silica (g) Inorganic powder (g) Oil (g) Fatty salts (g) polyol (g) hydrophilic hydrophobic Hydrophilic color pigment Hydrophobic color pigment Functional ingredient (synthetic fluorophlogopite) Hydrogenated polydecene Isononyl Anisononanoate Polyhydroxystearic acid Dipropylene glycol Example 1 5 65 30 Example 2 10 60 30 Example 3 10 60 30 Example 4 10 60 30 Example 5 10 60 15 15 Example 6 10 35 25 30 Example 7 10 59 30 One Example 8 10 40 19 30 One Example 9 10 60 30 Example 10 10 55 30 5 Example 11 10 35 20 30 5 Example 12 10 60 30 Comparative Example 1 One 70 30
  • Cosmetics were manufactured by adding the microcapsules prepared by the methods of Examples 1 to 12 and Comparative Example 1 to water-based cosmetics.
  • Examples 1 to 11 and Comparative Example 1 were color cosmetics, and Example 12 was manufactured as skin care cosmetics.
  • Sensory evaluation of unique feeling of use, adhesion, spreadability, coverage, and finish was conducted on 10 panelists with more than 3 years of cosmetics research experience. The evaluation results are shown in Table 2 below.
  • Examples 1 to 12 all have superior performance compared to Comparative Example 1.
  • Examples 7 to 8 in which microcapsules contain fatty acid salts, and Examples 10 to 11, in which microcapsules contain polyol, have high sensory evaluation scores.
  • fatty acid salts can stabilize the unstable interface between the hydrophilic inorganic powder and the hydrophobic oil to ensure a unique feeling of use and increase the viscosity of the cosmetic to improve adhesion.
  • the inorganic powder showing hydrophobic properties is complexed with the hydrophilic polyol, so that it can be mixed well without any discomfort even in water-based cosmetics, which is advantageous because it can improve the feeling of use and adhesion to the user.
  • Example 2 to 3 form microcapsules with high sphericity.
  • Figure 1(a) is an SEM image of a microcapsule prepared by the method of Example 2
  • Figure 1(b) is an SEM image of a microcapsule prepared by the method of Example 3.
  • both the microcapsules of Example 2 containing hydrophobic amorphous silica as a shell and Example 3 containing hydrophilic amorphous silica as a shell contain a high content of oil and inorganic powder in the core, and at the same time, the microcapsules It can be confirmed that it has high sphericity.
  • Figure 2 is an SEM image of a microcapsule manufactured by the method according to Comparative Example 1.
  • the microcapsule produced due to the low content of amorphous silica did not sufficiently surround the core material, so a spherical microcapsule was not formed and the capsule was broken. You can check that.
  • Figure 3 is a diagram showing an SEM image of microcapsules manufactured by the method according to Example 7. Referring to Figure 3, it can be seen that the hydrophilic inorganic powder was complexed with the fatty acid salt to form a rough surface of the microcapsule.
  • Figure 4(a) shows a microcapsule prepared according to Example 9
  • Figure 4(b) shows an SEM image of a microcapsule prepared according to Example 10.
  • Figure 4 in Examples 9 and 10, it can be seen that the surface of the microcapsules was roughened by using a hydrophobic color pigment as an inorganic powder.

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Abstract

This microcapsule comprises: a core containing an oil and an inorganic powder; and a shell that is disposed on the core and has a plurality of amorphous silica particles densely assembled, wherein the oil and the inorganic powder constitute 80-99 wt% of the total weight of the microcapsule, and the shell is porous. Accordingly, the microcapsule may contain a high content of oil and does not need to be aged, and thus can be applied to various types of cosmetics without becoming a source of irritation. Moreover, the microcapsule does not require additional additives to manufacture, and thus is unlikely to have harmful effects on the skin.

Description

고함량의 오일 및 무정형 실리카를 포함하는 마이크로캡슐 및 이의 제조방법Microcapsules containing high content of oil and amorphous silica and method for producing the same
본 발명은 고함량의 오일 및 무정형 실리카를 포함하는 마이크로캡슐 및 이의 제조방법에 관한 것으로, 보다 구체적으로 첨가제 없이 물리적인 방법으로 제조할 수 있는 마이크로캡슐 및 이의 제조방법에 관한 것이다. The present invention relates to microcapsules containing a high content of oil and amorphous silica and a method for producing the same, and more specifically, to a microcapsule that can be produced by a physical method without additives and a method for producing the same.
마이크로캡슐은 코어 및 상기 코어를 둘러싸는 쉘으로 구성되어, 불안정하거나 지속력이 약한 유효성분을 함유하는 코어물질을 쉘을 통해 보호하고, 적절한 때에 방출하는 특징을 가진다. 마이크로캡슐은 코어 물질의 종류에 따라 다양한 분야에 활용될 수 있는데, 특히 취급이 간편하고, 오일과 물처럼 잘 섞이지 않는 물질을 용이하게 혼합할 수 있어 화장료 분야에 활용도가 높다. Microcapsules are composed of a core and a shell surrounding the core, and have the characteristic of protecting the core material containing an unstable or weakly lasting active ingredient through the shell and releasing it at an appropriate time. Microcapsules can be used in a variety of fields depending on the type of core material. They are especially useful in the cosmetics field because they are easy to handle and can easily mix substances that do not mix well, such as oil and water.
종래에는 마이크로캡슐의 쉘로 고분자 또는 왁스를 사용하였다. 쉘로 고분자 또는 왁스를 사용하는 마이크로캡슐은 화장료 제형에 적용하기 까다로운 문제가 있다. 화장료의 제형이 달라질 때마다 쉘의 숙성 특성 또한 달라지기 때문에, 다양한 제형의 화장료에 범용적으로 적용하는 것이 어렵고, 숙성 특성에 의해 마이크로캡슐의 안정성이 저하될 수 있다. Previously, polymers or wax were used as the shell of microcapsules. Microcapsules that use polymers or wax as shells have a difficult problem when applied to cosmetic formulations. Since the maturation characteristics of the shell also change as the formulation of the cosmetic changes, it is difficult to universally apply it to cosmetics of various formulations, and the stability of the microcapsules may be reduced due to the maturation characteristics.
또한, 종래의 마이크로캡슐은 졸-겔법(sol-gel process) 및 계면 중합법 등의 화학적인 방법으로 제조하였다. 화학적 방법으로 마이크로캡슐을 제조하는 경우, 촉매, 표면처리제 및 계면활성제와 같은 첨가제가 필요하다. 첨가제를 사용하면 마이크로캡슐의 제조공정이 복잡해지고, 첨가제를 마이크로캡슐에서 제거하는 것이 어려워 제조된 마이크로캡슐이 첨가제를 포함할 수 있다. 첨가제를 포함하는 마이크로캡슐을 함유하는 화장료 조성물을 피부에 도포하는 경우, 발진, 두드러기 등의 피부 질환을 유발할 수 있어 안전성에 문제가 발생할 수 있다.In addition, conventional microcapsules were manufactured by chemical methods such as sol-gel process and interfacial polymerization. When producing microcapsules by chemical methods, additives such as catalysts, surface treatment agents, and surfactants are required. When additives are used, the manufacturing process of microcapsules becomes complicated, and it is difficult to remove the additives from the microcapsules, so the manufactured microcapsules may contain the additives. When a cosmetic composition containing microcapsules containing additives is applied to the skin, it may cause skin diseases such as rashes and hives, which may lead to safety issues.
이를 개선하기 위해 대한민국 공개특허공보 10-2015-0082870에서는 유화제 대신 분체인 폴리메틸메타크릴레이트(polymethylmethacrylate) 및 실리카 파우더를 사용한 피커링 에멀젼을 제조하였다. 그러나, 피커링 에멀젼은 수상부와 유상부의 계면 안정성을 유지하기가 어렵고, 산, 염기, 온도 등의 외부 환경 변화에 취약하여 에멀젼이 쉽게 파괴될 위험성이 있다.To improve this, Korean Patent Publication No. 10-2015-0082870 manufactured a Pickering emulsion using powdered polymethylmethacrylate and silica powder instead of an emulsifier. However, Pickering emulsion is difficult to maintain the stability of the interface between the water phase and the oil phase, and is vulnerable to external environmental changes such as acids, bases, and temperature, so there is a risk that the emulsion is easily destroyed.
따라서, 마이크로캡슐이 첨가제를 포함하지 않아 피부에 악영향을 미치지 않으며, 제조방법이 간단하고, 화장료의 제형에 영향을 받지 않아 다양한 제형의 화장료에 폭넓게 적용할 수 있는 마이크로캡슐에 대한 연구가 필요한 실정이다.Therefore, there is a need for research on microcapsules that do not contain additives and do not have a negative effect on the skin, have a simple manufacturing method, and are not affected by the formulation of the cosmetic, so they can be widely applied to various types of cosmetics. .
본 발명의 목적은 상기 종래 기술의 문제를 해결하기 위한 것으로서, 고함량의 오일을 함유하고, 제조 시 촉매, 표면처리제 및 계면활성제와 같은 첨가제가 요구되지 않는 마이크로캡슐 및 이의 제조방법을 제공하는 것이다.The purpose of the present invention is to solve the problems of the prior art, and to provide microcapsules that contain a high content of oil and do not require additives such as catalysts, surface treatment agents, and surfactants during production, and a method for producing the same. .
본 발명에 따른 마이크로캡슐은 오일 및 무기분체를 함유하는 코어 및 상기 코어 상에 위치하여 복수의 무정형 실리카 입자가 조밀하게 조립된 쉘을 포함하는 마이크로캡슐로서, 상기 마이크로캡슐의 총 중량에 대해 80 내지 99 중량%의 오일 및 무기분체를 포함하고, 상기 쉘은 다공성을 가지는 것을 특징으로 한다.The microcapsule according to the present invention is a microcapsule comprising a core containing oil and inorganic powder and a shell in which a plurality of amorphous silica particles are densely assembled located on the core, and is 80 to 80% based on the total weight of the microcapsule. It contains 99% by weight of oil and inorganic powder, and the shell is characterized by being porous.
일 실시예에 있어서, 상기 무정형 실리카 입자는 마이크로캡슐의 총 중량에 대해 1 내지 20 중량%를 포함할 수 있다.In one embodiment, the amorphous silica particles may contain 1 to 20% by weight based on the total weight of the microcapsule.
일 실시예에 있어서, 상기 무기분체의 중량이 상기 오일보다 더 많을 수 있다. In one embodiment, the weight of the inorganic powder may be greater than the oil.
일 실시예에 있어서, 상기 마이크로캡슐에 함유된 오일과 무기분체의 중량비는 1 : 1.5 내지 1 : 4일 수 있다.In one embodiment, the weight ratio of oil and inorganic powder contained in the microcapsules may be 1:1.5 to 1:4.
일 실시예에 있어서, 상기 무정형 실리카 입자의 평균입경(D50)은 400 내지 500 nm일 수 있다.In one embodiment, the average particle diameter (D 50 ) of the amorphous silica particles may be 400 to 500 nm.
일 실시예에 있어서, 상기 무정형 실리카 입자의 입도분포폭((D90-D10)/D50)은 0.9 내지 1.2일 수 있다.In one embodiment, the particle size distribution width ((D 90 -D 10 )/D 50 ) of the amorphous silica particles may be 0.9 to 1.2.
일 실시예에 있어서, 상기 쉘은 200 내지 800 nm 입경의 기공을 포함하는 다공성 쉘일 수 있다.In one embodiment, the shell may be a porous shell including pores with a particle diameter of 200 to 800 nm.
일 실시예에 있어서, 상기 마이크로캡슐의 평균입경은 30 내지 300 ㎛일 수 있다. In one embodiment, the average particle diameter of the microcapsules may be 30 to 300 ㎛.
일 실시예에 있어서, 상기 무기분체는 지방산염과 복합화된 친수성 무기분체를 포함할 수 있다.In one embodiment, the inorganic powder may include a hydrophilic inorganic powder complexed with a fatty acid salt.
일 실시예에 있어서, 상기 무기분체는 폴리올과 복합화된 소수성 무기분체를 포함할 수 있다.In one embodiment, the inorganic powder may include a hydrophobic inorganic powder complexed with polyol.
일 실시예에 있어서, 상기 무기분체는 이산화티탄, 산화철안료, 유기안료, 레이크염료, 천연안료, 합성플루오르플로고파이트, 산화아연, 질화붕소, 탈크, 카올린, 마이카, 견운모, 황산바륨, 판상알루미나, 펄 또는 이들의 혼합물을 포함할 수 있다.In one embodiment, the inorganic powder is titanium dioxide, iron oxide pigment, organic pigment, lake dye, natural pigment, synthetic fluorophlogopite, zinc oxide, boron nitride, talc, kaolin, mica, sericite, barium sulfate, and sheet alumina. , pearl, or mixtures thereof.
본 발명에 따른 화장료 조성물은 상기 마이크로캡슐을 함유할 수 있다.The cosmetic composition according to the present invention may contain the above microcapsules.
본 발명은 상술한 마이크로캡슐의 제조방법을 포함한다. The present invention includes the method for producing the above-described microcapsules.
본 발명에 따른 마이크로캡슐의 제조방법은 무정형 실리카 입자, 오일, 무기 분체 및 용매를 포함하는 분산액을 제조하는 단계; 및 상기 분산액을 회전 분무 건조기로 분무 건조하여 마이크로캡슐 입자를 제조하는 단계;를 포함하며, 상기 오일 및 무기분체는 상기 분산액의 총 중량에 대하여 10 내지 30 중량%를 함유한다.The method for producing microcapsules according to the present invention includes preparing a dispersion containing amorphous silica particles, oil, inorganic powder, and solvent; and spray-drying the dispersion using a rotary spray dryer to produce microcapsule particles, wherein the oil and inorganic powder contain 10 to 30% by weight based on the total weight of the dispersion.
일 실시예에 있어서, 상기 마이크로캡슐 입자를 체분급기에 통과하여 선별하는 단계를 더 포함할 수 있다.In one embodiment, the step of sorting the microcapsule particles by passing them through a sieve classifier may be further included.
일 실시예에 있어서, 상기 용매는 에탄올 및 아세톤을 포함하는 군에서 선택되는 하나를 포함할 수 있다.In one embodiment, the solvent may include one selected from the group including ethanol and acetone.
본 발명에 따른 마이크로캡슐은 화장료의 제형에 구애받지 않고, 다양한 제형에 적용할 수 있다. The microcapsule according to the present invention is not limited by the formulation of the cosmetic and can be applied to various formulations.
또한, 마이크로캡슐이 첨가제를 포함하지 않아 피부에 자극을 유발하지 않을 수 있다.Additionally, because the microcapsules do not contain additives, they may not cause skin irritation.
나아가, 마이크로캡슐이 고함량의 오일을 함유하여, 수분제형의 화장료에 적용하는 경우, 사용자에게 독특한 사용감 및 우수한 보습력을 제공할 수 있는 마이크로캡슐 및 이의 제조방법을 제공하는 것이다.Furthermore, the present invention provides a microcapsule that contains a high content of oil and can provide a unique feeling of use and excellent moisturizing power to the user when applied to a water-based cosmetic, and a method of manufacturing the same.
도 1은 실시예 2에 따른 방법으로 제조된 마이크로캡슐(a) 및 실시예 3에 따른 방법으로 제조된 마이크로캡슐(b)의 표면을 주사전자현미경(SEM)으로 관측한 사진이다.Figure 1 is a photograph of the surface of a microcapsule (a) manufactured by the method according to Example 2 and a microcapsule (b) manufactured by the method according to Example 3 observed with a scanning electron microscope (SEM).
도 2는 비교예 1에 따른 방법으로 제조된 마이크로캡슐의 표면을 주사전자현미경(SEM)으로 관측한 사진이다.Figure 2 is a photograph of the surface of a microcapsule manufactured by the method according to Comparative Example 1 observed with a scanning electron microscope (SEM).
도 3은 실시예 7에 따른 방법으로 제조된 마이크로캡슐의 표면을 주사전자현미경(SEM)으로 관측한 사진이다.Figure 3 is a photograph of the surface of a microcapsule manufactured by the method according to Example 7 observed with a scanning electron microscope (SEM).
도 4는 실시예 9에 따른 방법으로 제조된 마이크로캡슐(a) 및 실시예 10에 따른 방법으로 제조된 마이크로캡슐(b)의 표면을 주사전자현미경(SEM)으로 관측한 사진이다.Figure 4 is a photograph of the surface of a microcapsule (a) manufactured by the method according to Example 9 and a microcapsule (b) manufactured by the method according to Example 10 observed with a scanning electron microscope (SEM).
본 발명의 무정형 실리카를 포함하는 마이크로캡슐 및 이의 제조방법을 상세히 설명한다. 본 명세서에서 사용되는 용어는 본 발명의 기능을 고려하면서 가능한 현재 널리 사용되는 일반적인 용어들을 선택하였으나, 이는 관련 분야에 종사하는 기술자의 의도 또는 판례, 새로운 기술의 출현 등에 따라 달라질 수 있다. 사용되는 기술 용어 및 과학 용어에 있어서 다른 정의가 없다면, 이 발명이 속하는 기술 분야에서 통상의 지식을 가진 자가 통상적으로 이해하고 있는 의미를 가질 수 있다.The microcapsule containing amorphous silica of the present invention and its manufacturing method will be described in detail. The terms used in this specification are general terms that are currently widely used as much as possible while considering the function of the present invention, but this may vary depending on the intention or precedent of a technician working in the related field, the emergence of new technology, etc. Unless otherwise defined, the technical and scientific terms used may have meanings commonly understood by those skilled in the art in the technical field to which this invention belongs.
본 명세서 및 첨부된 특허청구범위에서 “포함하다” 또는 “가지다” 등의 용어는 명세서상에 기재된 특징, 또는 구성요소가 존재함을 의미하는 것이고, 특별히 한정하지 않는 한, 하나 이상의 다른 특징들 또는 구성요소가 부가될 가능성을 미리 배제하는 것은 아니다. In this specification and the appended patent claims, terms such as “include” or “have” mean the presence of features or components described in the specification, and, unless specifically limited, one or more other features or This does not preclude the possibility of additional components.
본 명세서 및 첨부된 특허청구범위에서 사용하는 단수의 표현은 문맥상 명백하게 단수인 것으로 특정하지 않는 한, 복수의 표현을 포함한다. 또한, 복수의 표현은 문맥상 명백하게 복수인 것으로 특정하지 않는 한, 단수의 표현을 포함한다.As used in this specification and the appended claims, singular expressions include plural expressions, unless the context clearly dictates the singular. Additionally, plural expressions include singular expressions, unless the context clearly specifies plural expressions.
또한, 본 명세서에서 사용되는 수치 범위는 하한치와 상한치와 그 범위 내에서의 모든 값, 정의되는 범위의 형태와 폭에서 논리적으로 유도되는 증분, 이중 한정된 모든 값 및 서로 다른 형태로 한정된 수치 범위의 상한 및 하한의 모든 가능한 조합을 포함한다. 본 발명의 명세서에서 특별한 정의가 없는 한 실험 오차 또는 값의 반올림으로 인해 발생할 가능성이 있는 수치범위 외의 값 역시 정의된 수치범위에 포함된다.In addition, the numerical range used in this specification includes the lower limit and upper limit and all values within the range, increments logically derived from the shape and width of the defined range, all double-defined values, and the upper limit of the numerical range defined in different forms. and all possible combinations of the lower bounds. Unless otherwise specified in the specification of the present invention, values outside the numerical range that may occur due to experimental error or rounding of values are also included in the defined numerical range.
본 명세서 및 첨부된 특허청구범위에서 사용되는 정도의 용어 "약" 등은 허용오차가 존재할 때 허용오차를 포괄하는 의미로 사용된 것이다.The terms "about" and the like used in this specification and the appended claims are used to encompass tolerance when tolerance exists.
본 발명에 따른 마이크로캡슐은 오일 및 무기분체를 함유하는 코어 및 상기 코어 상에 위치하여 복수의 무정형 실리카 입자가 조밀하게 조립된 쉘을 포함하며, 상기 마이크로캡슐의 총 중량에 대해 80 내지 99 중량%의 오일 및 무기분체를 포함하고, 상기 쉘은 다공성을 가진다.The microcapsule according to the present invention includes a core containing oil and inorganic powder and a shell in which a plurality of amorphous silica particles are densely assembled located on the core, and contains 80 to 99% by weight of the total weight of the microcapsule. of oil and inorganic powder, and the shell is porous.
오일 및 무기분체를 함유하는 코어 및 상기 코어를 둘러싸며, 복수의 무정형 실리카 입자가 조밀하게 조립된 쉘을 포함하는 코어-쉘 구조의 마이크로캡슐은 별도의 첨가제 없이도 우수한 안정성을 가질 수 있어 다양한 제형의 화장료에 폭넓게 적용할 수 있다. 또한, 높은 비표면적으로 코어에 포함된 오일 및 무기분체를 고함량으로 함유할 수 있는 장점이 있다.Microcapsules with a core-shell structure, which includes a core containing oil and inorganic powder and a shell surrounding the core and densely assembled with a plurality of amorphous silica particles, can have excellent stability without any additional additives and can be used in various formulations. It can be widely applied to cosmetics. In addition, it has the advantage of being able to contain a high content of oil and inorganic powder contained in the core due to its high specific surface area.
일반적으로 화장료에 사용되는 마이크로캡슐의 쉘로 유기 고분자 또는 왁스 등의 유기물질을 주로 사용하였다. 쉘로 유기물질을 함유하는 마이크로캡슐을 화장료에 적용할 때, 화장료의 제형에 따라 마이크로캡슐의 숙성 특성이 매번 달라져 숙성 조건이 까다로운 문제가 있다. 심지어 마이크로캡슐의 숙성 특성이 화장료의 제형과 적합하지 않은 경우, 마이크로캡슐을 함유하는 화장료의 사용감과 안정성이 극도로 저하될 수 있다. In general, organic materials such as organic polymers or wax are mainly used as the shell of microcapsules used in cosmetics. When applying microcapsules containing organic substances as shells to cosmetics, there is a problem in that the maturation conditions are difficult because the maturation characteristics of the microcapsules vary depending on the formulation of the cosmetic. Even if the ripening characteristics of the microcapsules are not suitable for the formulation of the cosmetic, the usability and stability of the cosmetic containing the microcapsules may be extremely reduced.
반면, 무기물질인 무정형 실리카는 화장료의 제형이 변화하여도 숙성 특성이 영향을 받지 않을 수 있으며, 보다 유리하게는 숙성 과정이 필요하지 않을 수 있다. 이에, 마이크로캡슐의 쉘이 무정형 실리카를 포함하는 경우, 화장료의 제형에 구애받지 않고 다양한 제형에서 뛰어난 사용감과 우수한 안정성을 가질 수 있어 범용성 측면에서 유리하다.On the other hand, the aging characteristics of amorphous silica, which is an inorganic material, may not be affected even if the formulation of the cosmetic is changed, and more advantageously, the aging process may not be necessary. Accordingly, when the shell of the microcapsule contains amorphous silica, it is advantageous in terms of versatility because it can have excellent feeling of use and excellent stability in various formulations regardless of the formulation of the cosmetic.
구체적으로, 마이크로캡슐의 쉘은 복수의 무정형 실리카 입자가 조밀하게 조립된 것일 수 있으며, 쉘을 형성하는 무정형 실리카 입자의 평균입경(D50)은 400 내지 500nm 또는 420 내지 480nm일 수 있으며, 바람직하게는 440 내지 460nm일 수 있다. 또는, 400nm 이상, 410nm 이상, 420nm 이상, 430nm 이상 또는 440nm 이상일 수 있으며, 상한으로는 500nm 이하, 490nm 이하, 480nm 이하, 470nm 이하, 460nm 이하 또는 450nm 이하일 수 있다. 상기 범위의 평균 입경을 갖는 무정형 실리카는 마이크로캡슐의 입경보다 현저하게 작은 입경을 갖고 있어 마이크로캡슐의 쉘에 무정형 실리카가 조밀하게 조립될 수 있다.Specifically, the shell of the microcapsule may be a dense assembly of a plurality of amorphous silica particles, and the average particle diameter (D 50 ) of the amorphous silica particles forming the shell may be 400 to 500 nm or 420 to 480 nm, preferably may be 440 to 460 nm. Alternatively, it may be 400 nm or more, 410 nm or more, 420 nm or more, 430 nm or more, or 440 nm or more, and the upper limit may be 500 nm or less, 490 nm or less, 480 nm or less, 470 nm or less, 460 nm or less, or 450 nm or less. Amorphous silica having an average particle size in the above range has a particle size that is significantly smaller than that of the microcapsule, so the amorphous silica can be densely assembled in the shell of the microcapsule.
일 실시예에 있어서, 상기 무정형 실리카 입자의 입도분포폭((D90-D10)/D50)은 0.90 내지 1.20, 0.94 내지 1.16, 또는 0.98 내지 1.12일 수 있으며, 바람직하게는 1.0 내지 1.10일 수 있다. 또는 0.90 이상, 0.92 이상, 0.94 이상, 0.96 이상, 0.98 이상 또는 1.0 이상일 수 있으며, 상한으로는 1.2 이하, 1.18 이하, 1.16 이하, 1.14 이하, 1.12 이하 또는 1.10 이하일 수 있다.In one embodiment, the particle size distribution width ((D 90 -D 10 )/D 50 ) of the amorphous silica particles may be 0.90 to 1.20, 0.94 to 1.16, or 0.98 to 1.12, and preferably 1.0 to 1.10 days. You can. Or it may be 0.90 or more, 0.92 or more, 0.94 or more, 0.96 or more, 0.98 or more, or 1.0 or more, and the upper limit may be 1.2 or less, 1.18 or less, 1.16 or less, 1.14 or less, 1.12 or less, or 1.10 or less.
입도분포폭은 하기의 식 1로 나타낼 수 있다.The particle size distribution width can be expressed in Equation 1 below.
[식 1][Equation 1]
입도분포폭 = (D90-D10)/D50 Particle size distribution width = (D 90 -D 10 )/D 50
상기 D90, D50 및 D10은 전체 무정형 실리카의 입경 분포에서, 누적 백분율이 각각 90%, 50%, 10%에 도달하였을 때, 무정형 실리카의 입경을 의미한다. 입도분포폭이 좁을수록 무정형 실리카의 입경의 크기 편차가 작은 단분산성의 입경 분포를 가질 수 있음을 의미한다.D 90 , D 50 , and D 10 refer to the particle size of amorphous silica when the cumulative percentage reaches 90%, 50%, and 10%, respectively, in the particle size distribution of the entire amorphous silica. A narrower particle size distribution means that amorphous silica can have a monodisperse particle size distribution with a smaller particle size deviation.
쉘에 포함된 복수의 무정형 실리카 입자들이 좁은 입도분포폭을 나타내어, 균일한 입자 크기를 가질 수 있다. 균일한 나노 사이즈의 무정형 실리카 입자가 마이크로캡슐의 쉘에 조밀하게 조립되어 보다 높은 구형도의 마이크로캡슐을 제조할 수 있어 유리하다. 높은 구형도를 갖는 마이크로캡슐은 표면의 질감이 거칠지 않고 매끄러운 표면을 가질 수 있어 피부에 도포 시, 이물감이 적고, 우수한 사용감을 제공할 수도 있다.A plurality of amorphous silica particles contained in the shell have a narrow particle size distribution width and can have a uniform particle size. It is advantageous because uniform nano-sized amorphous silica particles are densely assembled in the shell of the microcapsule, making it possible to manufacture microcapsules with higher sphericity. Microcapsules with high sphericity can have a smooth surface without a rough surface texture, so when applied to the skin, there is less foreign body sensation and can provide an excellent feeling of use.
일 실시예에 있어서, 복수의 무정형 실리카 입자 간의 빈 공간들에 의해 쉘은 다공성을 가질 수 있다. 구체적으로 쉘에 포함된 기공들의 평균 입경은 200 내지 800nm, 250 내지 750nm, 300 내지 700nm, 350 내지 650nm 또는 400 내지 600nm일 수 있다. 또는, 200nm 이상, 250nm 이상, 300nm 이상, 350nm 이상 또는 400nm 이상일 수 있으며, 상한으로는 800nm 이하, 750nm 이하, 700nm 이하, 650nm 이하 또는 600nm 이하일 수 있다. In one embodiment, the shell may have porosity due to empty spaces between a plurality of amorphous silica particles. Specifically, the average particle diameter of the pores included in the shell may be 200 to 800 nm, 250 to 750 nm, 300 to 700 nm, 350 to 650 nm, or 400 to 600 nm. Alternatively, it may be 200 nm or more, 250 nm or more, 300 nm or more, 350 nm or more, or 400 nm or more, and the upper limit may be 800 nm or less, 750 nm or less, 700 nm or less, 650 nm or less, or 600 nm or less.
마이크로캡슐의 쉘이 상기 입경 범위를 갖는 기공들을 포함하여 표면적을 향상시킬 수 있다. 쉘의 표면적이 증가함에 따라, 마이크로캡슐의 코어에 많은 양의 오일을 함유할 수 있다. 또한, 오일을 마이크로캡슐의 외부로 방출할 때, 브러쉬 또는 손을 사용해 마이크로캡슐에 작은 충격을 가하는 것만으로도 다공성의 쉘이 쉽게 파괴되어 코어 물질을 용이하게 방출시킬 수 있다. The shell of the microcapsule may include pores having the above particle size range to improve the surface area. As the surface area of the shell increases, the core of the microcapsule can contain a larger amount of oil. Additionally, when releasing oil to the outside of the microcapsule, the porous shell can be easily destroyed by simply applying a small impact to the microcapsule using a brush or hand, allowing the core material to be easily released.
쉘이 높은 표면적을 갖는 무정형 실리카를 포함하여, 마이크로캡슐이 우수한 표면적을 가질 수 있다. 따라서, 무정형 실리카가 다량의 오일을 흡수하여 마이크로캡슐의 코어에 더 많은 양의 오일을 담지할 수 있어 유리하다.If the shell contains amorphous silica with a high surface area, the microcapsules can have excellent surface area. Therefore, it is advantageous because amorphous silica can absorb a large amount of oil and support a larger amount of oil in the core of the microcapsule.
구체적으로, 무정형 실리카의 BET 표면적은 100 내지 200m2/g, 110 내지 190m2/g 또는 120 내지 180m2/g일 수 있으며, 실질적으로 125 내지 175m2/g일 수 있다. 또는, 100m2/g 이상, 105m2/g 이상, 110m2/g 이상, 115m2/g 이상, 120m2/g 이상 또는 125m2/g 이상일 수 있으며, 상한으로는 200m2/g 이하, 195m2/g 이하, 190m2/g 이하, 185m2/g 이하 또는 180m2/g 이하 또는 175m2/g 이하일 수 있다.Specifically, the BET surface area of amorphous silica may be 100 to 200 m 2 /g, 110 to 190 m 2 /g, or 120 to 180 m 2 /g, and may be substantially 125 to 175 m 2 /g. Alternatively, it may be 100 m 2 /g or more, 105 m 2 /g or more, 110 m 2 /g or more, 115 m 2 /g or more, 120 m 2 /g or more, or 125 m 2 /g or more, with the upper limit being 200 m 2 /g or less, 195 m 2 /g or less, 190 m 2 /g or less, 185 m 2 /g or less, or 180 m 2 /g or less, or 175 m 2 /g or less.
일 실시예에 있어서, 무정형 실리카는 마이크로캡슐의 총 중량에 대해 1 내지 20 중량%, 3 내지 18 중량%, 5 내지 16 중량%, 7 내지 14 중량% 및 9 내지 12 중량%를 포함할 수 있다. 마이크로캡슐이 넓은 표면적을 갖는 무정형 실리카를 상기 중량비로 포함하여, 무정형 실리카의 중량이 코어물질의 중량보다 현저히 적어도, 효과적으로 코어 물질을 감쌀 수 있어 용이하게 구형의 마이크로캡슐을 제조할 수 있다.In one embodiment, the amorphous silica may comprise 1 to 20%, 3 to 18%, 5 to 16%, 7 to 14% and 9 to 12% by weight relative to the total weight of the microcapsule. . Since the microcapsule contains amorphous silica with a large surface area in the above weight ratio, the weight of the amorphous silica is significantly less than that of the core material, but it can effectively surround the core material, making it possible to easily manufacture spherical microcapsules.
마이크로캡슐이 상기 범위보다 적은 중량%의 무정형 실리카를 함유하는 경우, 코어물질을 충분히 감싸지 못해 마이크로캡슐의 안정성이 저하될 수 있으며, 상기 범위보다 많은 중량%의 무정형 실리카를 함유하는 경우, 점도가 상승하여 구형도가 낮은 마이크로캡슐이 제조되어 사용감이 저하될 우려가 있다.If the microcapsule contains less amorphous silica by weight than the above range, the stability of the microcapsule may be reduced due to insufficient envelopment of the core material, and if it contains amorphous silica of more weight% than the above range, the viscosity increases. As a result, there is a risk that microcapsules with low sphericity may be produced and the feeling of use may be reduced.
일 실시예에 있어서, 마이크로캡슐의 코어물질인 오일 및 무기분체는 마이크로캡슐의 총 중량에 대해 80 내지 99 중량%, 82 내지 97 중량%, 84 내지 95 중량%, 84 내지 93 중량% 및 85 내지 90 중량%을 함유할 수 있다. 마이크로캡슐의 쉘에 포함된 무정형 실리카가 넓은 표면적을 가질 뿐만 아니라 오일 흡수성이 좋아, 쉘의 중량 대비 다량의 오일을 마이크로캡슐의 코어에 함유할 수 있다.In one embodiment, the oil and inorganic powder, which are the core materials of the microcapsule, are 80 to 99% by weight, 82 to 97% by weight, 84 to 95% by weight, 84 to 93% by weight, and 85 to 85% by weight, based on the total weight of the microcapsule. It may contain 90% by weight. The amorphous silica contained in the shell of the microcapsule not only has a large surface area but also has good oil absorption, so a large amount of oil can be contained in the core of the microcapsule compared to the weight of the shell.
일 구체예에 있어서, 오일보다 무기분체의 중량이 더 많을 수 있다. 마이크로캡슐에 함유된 오일과 무기분체의 중량비는 1 : 1.5 내지 4, 1 : 1.6 내지 3.8, 1 : 1.7 내지 3.5 및 1 : 1.8 내지 3.2일 수 있으며, 바람직하게는 1 : 1.8 내지 3.0 일 수 있다. 상술한 바와 같이, 코어 쉘 구조를 갖는 마이크로캡슐은 오일보다 무기분체를 더 많은 중량으로 포함할 수 있어 화장료 조성물에 적용 시 성능을 향상시킬 수 있다. 일 예로, 무기분체가 색조 안료를 상기 중량비로 포함하는 경우, 색 발현 시 채도가 낮아지지 않고 선명한 발색력을 나타낼 수 있다. 무기분체가 기능성 분체를 포함하는 경우, 우수한 커버력, 발림성 및 자외선 차단 효과를 가질 수 있다.In one embodiment, the weight of the inorganic powder may be greater than that of the oil. The weight ratio of oil and inorganic powder contained in the microcapsule may be 1:1.5 to 4, 1:1.6 to 3.8, 1:1.7 to 3.5, and 1:1.8 to 3.2, and preferably 1:1.8 to 3.0. . As described above, microcapsules with a core-shell structure can contain more inorganic powder by weight than oil, which can improve performance when applied to cosmetic compositions. For example, when the inorganic powder contains a color pigment in the above weight ratio, vivid color development can be achieved without lowering saturation during color development. When the inorganic powder includes functional powder, it can have excellent covering power, spreadability, and ultraviolet ray blocking effects.
마이크로캡슐의 평균 입경은 30 내지 300㎛, 60 내지 250㎛, 90 내지 200㎛ 또는 100 내지 180㎛일 수 있다. 또는 30㎛ 이상, 50㎛ 이상, 70㎛ 이상, 90㎛ 이상 또는 100㎛ 이상일 수 있으며, 상한으로는 300㎛ 이하, 250㎛ 이하, 230㎛ 이하, 200㎛ 이하 또는 180㎛ 이하일 수 있다. 본 발명이 마이크로캡슐의 평균 입경에 의해 한정되는 것은 아니나, 상기 입경 범위를 갖는 마이크로캡슐을 피부에 도포할 때, 이질감이 적어 우수한 사용감을 제공할 수 있어 유리하다. The average particle diameter of the microcapsule may be 30 to 300 μm, 60 to 250 μm, 90 to 200 μm, or 100 to 180 μm. Alternatively, it may be 30 μm or more, 50 μm or more, 70 μm or more, 90 μm or more, or 100 μm or more, and the upper limit may be 300 μm or less, 250 μm or less, 230 μm or less, 200 μm or less, or 180 μm or less. Although the present invention is not limited by the average particle size of the microcapsules, it is advantageous because it provides an excellent feeling of use due to less heterogeneity when applying microcapsules having the above particle size range to the skin.
일 실시예에 있어서, 무기분체의 표면이 친수성을 나타낼 경우, 첨가제로 지방산염을 더 함유하여 마이크로캡슐이 지방산염과 복합화된 무기분체를 포함할 수 있다. 마이크로캡슐의 코어물질인 친수성인 무기분체와 오일이 서로 섞이지 않아 불안정한 상태를 형성할 수 있다. 그러나 마이크로캡슐에 지방산염을 첨가하여 무기분체와 오일간의 불안정한 계면을 안정화할 수 있다. 또한, 지방산염은 비수용성 점증제로 작용하여 화장료의 점도를 증가시켜 밀착감이 향상되는 효과를 제공할 수도 있다.In one embodiment, when the surface of the inorganic powder exhibits hydrophilicity, fatty acid salts may be further included as an additive so that the microcapsules may contain the inorganic powder complexed with the fatty acid salts. Hydrophilic inorganic powder, which is the core material of microcapsules, and oil do not mix with each other, which can form an unstable state. However, the unstable interface between inorganic powder and oil can be stabilized by adding fatty acid salts to microcapsules. In addition, fatty acid salts may act as a water-insoluble thickener to increase the viscosity of cosmetics and improve adhesion.
구체적으로 지방산염은 폴리하이드록시스테아릭애씨드, 마그네슘스테아레이트, 알루미늄스테아레이트, 칼슘라우레이트, 칼슘미리스테이트 및 마그네슘팔미테이트를 포함하는 군에서 선택되는 하나 이상을 포함할 수 있다.Specifically, the fatty acid salt may include one or more selected from the group including polyhydroxystearic acid, magnesium stearate, aluminum stearate, calcium laurate, calcium myristate, and magnesium palmitate.
일 실시예에 있어서, 무기분체의 표면이 소수성일 경우, 첨가제로 폴리올을 더 함유하여 마이크로캡슐이 폴리올과 복합화된 소수성 무기분체를 포함할 수 있다. 폴리올은 하이드록시기를 함유하고 있어 물에 잘 녹지 않는 고체성분을 녹일 수 있다. 폴리올과 복합화된 소수성 무기분체를 함유하는 마이크로캡슐을 수분제형에 첨가하여 사용할 때, 마이크로캡슐이 깨지면서 폴리올에 의해 소수성 무기분체가 수분제형과 이질감 없이 섞일 수 있다. 따라서, 화장료의 발림성 및 퍼짐성을 향상시키는 효과를 제공할 수 있다.In one embodiment, when the surface of the inorganic powder is hydrophobic, polyol may be further included as an additive, so that the microcapsules may include the hydrophobic inorganic powder complexed with the polyol. Polyol contains hydroxyl groups, so it can dissolve solid components that are not easily soluble in water. When microcapsules containing hydrophobic inorganic powder complexed with polyol are added to the water formulation, the microcapsules are broken and the hydrophobic inorganic powder can be mixed with the water formulation without any discomfort due to the polyol. Therefore, it can provide the effect of improving the applicability and spreadability of cosmetics.
폴리올은 다이프로필렌글리콜, 1,3-부탄디올, 에틸렌글리콜, 폴리에틸렌글리콜, 다이에틸렌글리콜, 글리세린, 펜틸렌글리콜, 솔비톨, 프로판디올 및 프로필렌글리콜을 포함하는 군에서 선택되는 하나 이상을 포함할 수 있다.The polyol may include one or more selected from the group including dipropylene glycol, 1,3-butanediol, ethylene glycol, polyethylene glycol, diethylene glycol, glycerin, pentylene glycol, sorbitol, propanediol, and propylene glycol.
일 실시예에 있어서, 무정형 실리카는 화장료 조성물의 종류에 따라 친수성 또는 소수성 실리카를 포함할 수 있다.In one embodiment, the amorphous silica may include hydrophilic or hydrophobic silica depending on the type of cosmetic composition.
일 실시예에 있어서, 오일은 하이드로카본계 오일, 에스테르계 오일 및 천연 오일을 포함하는 군에서 선택되는 하나 이상을 포함할 수 있다. 구체적으로 하이드로카본계 오일은 폴리부텐, 하이드로제네이티드폴리이소부텐 및 하이드로제네이티드폴리데센을 포함하는 군에서 선택되는 하나 이상을 포함할 수 있다.In one embodiment, the oil may include one or more selected from the group including hydrocarbon-based oil, ester-based oil, and natural oil. Specifically, the hydrocarbon-based oil may include one or more selected from the group including polybutene, hydrogenated polyisobutene, and hydrogenated polydecene.
에스테르계 오일은 세틸에틸헥사노에이트, 아이소세틸에틸헥사노에이트, 아이소세틸미리스테이트, 아이소프로필미리스테이트, 네오펜틸글라이콜다이카프레이트, 헥실라우레이트, 트리에틸헥사노인, 에틸헥실팔미테이트 및 아이소노닐아이소노나노에이트를 포함하는 군에서 선택되는 하나 이상을 포함할 수 있다.Ester oils include cetyl ethyl hexanoate, isocetyl ethyl hexanoate, isocetyl myristate, isopropyl myristate, neopentyl glycol dicaprate, hexyl laurate, triethylhexanoin, ethylhexyl palmitate, and It may include one or more selected from the group containing isononyl isononanoate.
천연 오일은 호호바 오일, 해바라기씨 오일, 아보카도 오일, 마카다미아씨 오일, MCT oil, 올리브 오일, 녹차씨 오일, 코코넛 오일, 유자 오일, 로즈힙 오일, 아르간 오일, 동백오일, 햄프씨드 오일, 달맞이 오일 및 살구 오일을 포함하는 군에서 선택되는 하나 이상의 식물성 오일 또는 유동 파라핀, 바셀린 및 실리콘 오일을 포함하는 군에서 선택되는 하나 이상의 광물성 오일을 포함할 수 있다.Natural oils include jojoba oil, sunflower seed oil, avocado oil, macadamia seed oil, MCT oil, olive oil, green tea seed oil, coconut oil, citron oil, rosehip oil, argan oil, camellia oil, hemp seed oil, evening primrose oil and apricot oil. It may include one or more vegetable oils selected from the group containing oils, or one or more mineral oils selected from the group containing liquid paraffin, petrolatum, and silicone oil.
무기분체는 화장료의 사용감을 향상시켜주는 기능성 분체 및 색상을 부여하는 색조 안료를 포함할 수 있다.Inorganic powders may include functional powders that improve the feeling of use of cosmetics and color pigments that provide color.
구체적으로 기능성 분체는 합성플루오르플로고파이트, 산화아연, 질화붕소, 탈크, 카올린, 마이카, 견운모, 황산바륨, 판상알루미나 및 펄을 포함하는 군에서 선택되는 하나 이상을 포함할 수 있다. 색조 안료는 이산화티탄, 산화철안료, 유기안료, 레이크염료 및 천연안료를 포함하는 군에서 선택되는 하나 이상을 포함할 수 있으나, 본 발명이 마이크로캡슐의 코어물질의 구체 종류에 의해 한정되는 것은 아니다. Specifically, the functional powder may include one or more selected from the group including synthetic fluorophlogopite, zinc oxide, boron nitride, talc, kaolin, mica, sericite, barium sulfate, sheet alumina, and pearl. The color pigment may include one or more selected from the group including titanium dioxide, iron oxide pigment, organic pigment, lake dye, and natural pigment, but the present invention is not limited by the specific type of the core material of the microcapsule.
본 발명에 따른 화장료 조성물은 상술한 마이크로캡슐을 함유할 수 있다. The cosmetic composition according to the present invention may contain the above-described microcapsules.
마이크로캡슐의 쉘로 무기물질인 무정형 실리카를 사용함으로써, 화장료의 제형이 변화하여도 마이크로캡슐의 숙성 특성이 변화하지 않을 수 있다. 따라서, 상술한 마이크로캡슐은 화장료의 제형에 제한되지 않고 다양한 제형의 화장료에 폭넓게 적용할 수 있어 유리하다.By using amorphous silica, an inorganic material, as the shell of the microcapsule, the aging characteristics of the microcapsule may not change even if the formulation of the cosmetic product changes. Therefore, the above-mentioned microcapsules are advantageous because they are not limited to the formulation of cosmetics and can be widely applied to various formulations of cosmetics.
또한, 쉘의 표면적이 커 다량의 오일을 담지할 수 있는 무정형 실리카를 포함하여 고함량의 오일을 함유하는 마이크로캡슐을 형성할 수 있다. 고함량의 오일을 함유하는 마이크로캡슐을 포함하는 수분제형의 화장료는 우수한 보습력을 가질 수 있으며, 마이크로캡슐의 코어에 다양한 무기분체를 함유하여 밀착력, 발림성을 향상시킬 수 있다.In addition, the shell has a large surface area, making it possible to form microcapsules containing a high content of oil, including amorphous silica, which can support a large amount of oil. Water-based cosmetics containing microcapsules containing a high content of oil can have excellent moisturizing power and can improve adhesion and spreadability by containing various inorganic powders in the core of the microcapsules.
특히 상술한 마이크로캡슐을 함유하는 화장료 조성물을 피부에 도포하는 경우, 마이크로캡슐에 충격을 가해 쉘이 파괴되어 코어 물질이 방출될 때, 친수성의 화장료 제형과 소수성의 오일이 서로 반발하면서 사용자에게 독특한 사용감을 부여할 수도 있다. In particular, when a cosmetic composition containing the above-mentioned microcapsules is applied to the skin, when impact is applied to the microcapsules and the shell is broken and the core material is released, the hydrophilic cosmetic formulation and the hydrophobic oil repel each other, giving the user a unique feeling of use. can also be given.
구체적으로, 화장료 조성물은 유연화장수, 수렴화장수, 영양화장수, 영양크림, 마사지크림, 에센스, 아이크림, 아이에센스, 클렌징크림, 클렌징폼, 클렌징워터, 팩, 파우더, 바디로션, 바디크림, 바디오일 및 자외선 차단제를 포함하는 군에서 선택되는 하나의 스킨케어 화장료에 적용할 수 있다. 또는, 메이크업 베이스, 파운데이션, 립스틱, 립글로스, 페이스파우더, 투웨이케익, 아이섀도 및 블러셔를 포함하는 군에서 선택되는 하나의 색조 화장료에도 적용할 수 있으나, 본 발명이 화장료의 구체 종류에 의해 한정되는 것은 아니다.Specifically, cosmetic compositions include softening lotion, astringent lotion, nourishing lotion, nourishing cream, massage cream, essence, eye cream, eye essence, cleansing cream, cleansing foam, cleansing water, pack, powder, body lotion, body cream, and body oil. And it can be applied to one skin care cosmetic selected from the group containing sunscreen. Alternatively, it can be applied to one color cosmetic selected from the group including makeup base, foundation, lipstick, lip gloss, face powder, two-way cake, eye shadow, and blusher, but the present invention is not limited by the specific type of cosmetic. no.
마이크로캡슐의 제조방법을 상술함에 있어, 코어 및 쉘의 물질, 구조 및 형상이나 크기 등은 앞서 상술한 마이크로캡슐과 동일 내지 유사함에 따라, 본 발명에 따른 마이크로캡슐의 제조방법은 앞서 마이크로캡슐에서 상술한 모든 내용을 포함한다.In detailing the manufacturing method of microcapsules, the material, structure, shape, size, etc. of the core and shell are the same or similar to the microcapsules described above, so the manufacturing method of microcapsules according to the present invention is described in detail in the microcapsules previously. Includes all contents.
본 발명에 따른 마이크로캡슐의 제조방법은 무정형 실리카 입자, 오일, 무기 분체 및 용매를 포함하는 분산액을 제조하는 단계; 및 상기 분산액을 회전 분무 건조기로 분무 건조하여 마이크로캡슐 입자를 제조하는 단계;를 포함하며, 상기 오일 및 무기분체는 상기 분산액의 총 중량에 대하여 10 내지 30 중량%를 함유할 수 있다.The method for producing microcapsules according to the present invention includes preparing a dispersion containing amorphous silica particles, oil, inorganic powder, and solvent; and preparing microcapsule particles by spray drying the dispersion using a rotary spray dryer, wherein the oil and inorganic powder may contain 10 to 30% by weight based on the total weight of the dispersion.
벽재물질로 무정형 실리카를 사용하는 마이크로캡슐의 제조 시, 종래에는 졸겔법 또는 모노머 합성 등 화학적인 방법으로 캡슐화를 수행하였다. 화학적인 방법으로 마이크로캡슐을 제조할 경우, 촉매, 표면처리제, 계면활성제 등 다량의 첨가제가 필요하다. 첨가제를 사용하는 경우, 마이크로캡슐의 제조공정이 복잡해지고, 첨가제를 제거하는 과정에서 다량의 폐수가 배출될 수도 있다. 또한, 마이크로캡슐에서 첨가제가 쉽게 제거되지 않아 제조된 마이크로캡슐에 첨가제가 잔존할 수 있다. 잔존 첨가제를 포함하는 마이크로캡슐을 피부에 도포할 경우, 첨가제가 피부에 자극을 유발하여 발진, 두드러기 등의 피부 질환이 발병할 위험이 있다.When manufacturing microcapsules using amorphous silica as a wall material, encapsulation was conventionally performed by chemical methods such as the sol-gel method or monomer synthesis. When manufacturing microcapsules by chemical methods, a large amount of additives such as catalysts, surface treatment agents, and surfactants are required. When additives are used, the manufacturing process of microcapsules becomes complicated, and a large amount of waste water may be discharged during the process of removing the additives. Additionally, since additives are not easily removed from microcapsules, additives may remain in the manufactured microcapsules. When microcapsules containing residual additives are applied to the skin, there is a risk that the additives may cause skin irritation and cause skin diseases such as rashes and hives.
본 발명에 따른 제조방법으로 마이크로캡슐을 제조하는 경우, 물리적인 방법으로 마이크로캡슐을 제조하여 최종 제품의 물성을 제어하는 것이 용이하고, 제조공정에서 첨가제를 사용하지 않고 간단한 제조공정으로 다량의 오일을 함유하는 마이크로캡슐을 제조할 수 있다.When manufacturing microcapsules using the manufacturing method according to the present invention, it is easy to control the physical properties of the final product by manufacturing the microcapsules by a physical method, and a large amount of oil can be produced through a simple manufacturing process without using additives in the manufacturing process. Microcapsules containing it can be manufactured.
상기 용매는 극성 용매로서, 에탄올 및 아세톤 중에서 선택되는 하나를 포함할 수 있다.The solvent is a polar solvent and may include one selected from ethanol and acetone.
휘발성이 높은 극성 용매를 사용하여 후술하는 분무 건조 단계에서 짧은 시간 내에 용매를 빠르게 건조할 수 있다. 열에 약한 마이크로캡슐이 고온에 노출되는 시간을 단축하여, 높은 구형도를 갖는 마이크로캡슐을 제조할 수 있다.By using a highly volatile polar solvent, the solvent can be dried quickly within a short time in the spray drying step described later. By shortening the exposure time of heat-sensitive microcapsules to high temperatures, microcapsules with high sphericity can be manufactured.
구체적으로, 상기 오일 및 무기분체는 상기 분산액의 총 중량에 대하여 10 내지 30 중량%, 12 내지 29 중량%, 14 내지 28 중량%, 16 내지 27 중량% 또는 18 내지 26 중량%를 함유할 수 있다. 또는 10 중량% 이상, 12 중량% 이상, 14 중량% 이상, 16 중량% 이상, 18 중량% 이상, 20 중량% 이상, 22 중량% 이상 또는 24 중량% 이상을 함유할 수 있으며, 상한으로는 30 중량% 이하, 29 중량% 이하, 28 중량% 이하, 27 중량% 이하, 26 중량% 이하 또는 25 중량% 이하로 오일 및 무기분체를 함유할 수 있다. 오일 및 무기분체를 상기 범위의 중량비로 첨가하여, 제조된 마이크로캡슐의 코어에 고함량의 오일과 무기분체가 함유될 수 있다.Specifically, the oil and inorganic powder may contain 10 to 30% by weight, 12 to 29% by weight, 14 to 28% by weight, 16 to 27% by weight, or 18 to 26% by weight based on the total weight of the dispersion. . Or it may contain 10% by weight or more, 12% by weight or more, 14% by weight or more, 16% by weight or more, 18% by weight or more, 20% by weight or more, 22% by weight or more, or 24% by weight or more, with an upper limit of 30% by weight. It may contain oil and inorganic powder in an amount of less than 29% by weight, less than 28% by weight, less than 27% by weight, less than 26% by weight, or less than 25% by weight. By adding oil and inorganic powder in a weight ratio within the above range, the core of the manufactured microcapsule can contain a high content of oil and inorganic powder.
제조된 분산액을 회전 분무 건조기에서 건조하여 분산액 내의 용매를 제거하면 마이크로캡슐을 제조할 수 있다. Microcapsules can be prepared by drying the prepared dispersion in a rotary spray dryer to remove the solvent in the dispersion.
일 실시예에 있어서, 회전 분무 건조기의 공급 온도는 용매의 비점보다 1 내지 50℃, 3 내지 40℃, 5 내지 30℃, 10 내지 25℃ 또는 10 내지 20℃ 높을 수 있다. 상기 온도 범위에서, 분산액에 포함된 용매를 단시간에 증발시켜 마이크로캡슐을 제조할 수 있다.In one embodiment, the feed temperature to the rotary spray dryer may be 1 to 50°C, 3 to 40°C, 5 to 30°C, 10 to 25°C, or 10 to 20°C above the boiling point of the solvent. In the above temperature range, microcapsules can be manufactured by evaporating the solvent contained in the dispersion in a short time.
본 발명에 따른 방법으로 마이크로캡슐을 제조하는 경우, 용매에 오일, 무정형 실리카, 무기분체를 분산시킨 분산액을 분무 건조기로 건조하는 간단한 공정으로 마이크로캡슐을 제조함으로써, 계면활성제를 비롯한 첨가제의 사용량 및 폐수의 배출량을 효과적으로 감축할 수 있다. 따라서, 비용 절감 및 친환경적인 공정을 제공할 수 있어 유리하다.When manufacturing microcapsules by the method according to the present invention, the microcapsules are manufactured through a simple process of drying a dispersion of oil, amorphous silica, and inorganic powder in a solvent with a spray dryer, thereby reducing the amount of additives used, including surfactants, and wastewater. emissions can be effectively reduced. Therefore, it is advantageous to reduce costs and provide an environmentally friendly process.
일 실시예에 있어서, 분무 건조 단계를 통해 제조한 마이크로캡슐을 체분급기에 통과하여 마이크로캡슐 입자를 선별하는 단계;를 더 포함할 수 있다.In one embodiment, the method may further include passing the microcapsules prepared through the spray drying step through a sieve classifier to select microcapsule particles.
체분급기를 통해 500㎛ 이하, 450㎛ 이하, 400㎛ 이하, 350㎛ 이하 또는 300㎛ 이하의 입경을 갖는 마이크로캡슐을 선별할 수 있다. 상기 범위의 입경을 갖는 마이크로캡슐을 선별하여 화장료 제형에 적용하였을 때, 제형과의 이질감 없이 사용감을 향상시킬 수 있다.Microcapsules having a particle size of 500 ㎛ or less, 450 ㎛ or less, 400 ㎛ or less, 350 ㎛ or less, or 300 ㎛ or less can be selected through a sieve classifier. When microcapsules with a particle size within the above range are selected and applied to a cosmetic formulation, the feeling of use can be improved without any feeling of incompatibility with the formulation.
이하, 실시예 및 비교예를 통해 본 발명을 더욱 상세히 설명한다.Hereinafter, the present invention will be described in more detail through examples and comparative examples.
(실시예 1)(Example 1)
유기용매인 에탄올 257g에 소수성 무정형 실리카 5g, 무기분체로 이산화티탄, 옐로우산화철, 레드산화철, 블랙산화철을 9.0:0.7:0.2:0.1 비율로 배합한 친수성 색조안료 65g, 오일로 하이드로제네이티드폴리데센 30g을 교반시켜 균질하게 혼합한 분산액을 제조하였다. 상기 분산액을 3500rpm으로 회전하는 회전 분무 건조기로 투입하여 분산액을 분무 건조시켜 마이크로캡슐을 제조하였다. 이때, 분무 건조기의 공급 온도는 80℃이고, 분무 건조기의 내부 온도는 60℃이다. 상기 마이크로캡슐을 체분급기에 통과시켜 외부입경이 300㎛이하인 마이크로캡슐을 선별하였다.257g of ethanol as an organic solvent, 5g of hydrophobic amorphous silica, 65g of hydrophilic color pigment mixed with titanium dioxide, yellow iron oxide, red iron oxide, and black iron oxide as inorganic powder in a ratio of 9.0:0.7:0.2:0.1, and 30g of hydrogenated polydecene as oil. was stirred to prepare a homogeneously mixed dispersion. The dispersion was put into a rotary spray dryer rotating at 3500 rpm and the dispersion was spray dried to prepare microcapsules. At this time, the supply temperature of the spray dryer is 80°C, and the internal temperature of the spray dryer is 60°C. The microcapsules were passed through a sieve sorter to select microcapsules with an external particle diameter of 300 ㎛ or less.
(실시예 2)(Example 2)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 친수성 색조안료 60g, 오일로 하이드로제네이티드폴리데센 30g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of hydrophilic color pigment as inorganic powder, and 30 g of hydrogenated polydecene as oil were added.
(실시예 3)(Example 3)
분산액 제조 시, 친수성 무정형 실리카 10g, 무기분체로 친수성 색조안료 60g, 오일로 하이드로제네이티드폴리데센 30g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophilic amorphous silica, 60 g of hydrophilic color pigment as inorganic powder, and 30 g of hydrogenated polydecene as oil were added.
(실시예 4)(Example 4)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 친수성 색조안료 60g, 오일로 아이소노닐아이소노나노에이트 30g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of hydrophilic color pigment as inorganic powder, and 30 g of isononyl isononanoate as oil were added.
(실시예 5)(Example 5)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 친수성 색조안료 60g, 오일로 하이드로제네이티드폴리데센 15g, 아이소노닐아이소노나노에이트 15g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of hydrophilic color pigment as inorganic powder, 15 g of oil-hydrogenated polydecene, and 15 g of isononyl isononanoate were added. was manufactured.
(실시예 6)(Example 6)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 친수성 색조안료 35g, 합성플루오르플로고파이트 25g, 오일로 하이드로제네이티드폴리데센 30g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 35 g of hydrophilic color pigment as inorganic powder, 25 g of synthetic fluorophlogopite, and 30 g of oil-hydrogenated polydecene were added. did.
(실시예 7)(Example 7)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 친수성 색조안료 59g, 오일로 하이드로제네이티드폴리데센 30g 및 지방산염으로 폴리하이드록시스테아릭애씨드 1g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, 10 g of hydrophobic amorphous silica, 59 g of hydrophilic color pigment as inorganic powder, 30 g of hydrogenated polydecene as oil, and 1 g of polyhydroxystearic acid as fatty acid salt were added in the same manner as Example 1. Microcapsules were prepared.
(실시예 8)(Example 8)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 친수성 색조안료 40g, 합성플루오르플로고파이트 19g, 오일로 하이드로제네이티드폴리데센 30g 및 지방산염으로 폴리하이드록시스테아릭애씨드 1g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, 10 g of hydrophobic amorphous silica, 40 g of hydrophilic color pigment as inorganic powder, 19 g of synthetic fluorophlogopite, 30 g of oil-hydrogenated polydecene, and 1 g of polyhydroxystearic acid as a fatty acid salt were added. Microcapsules were prepared in the same manner as in Example 1.
(실시예 9)(Example 9)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 소수성 색조안료 60g, 오일로 하이드로제네이티드폴리데센 30g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of hydrophobic color pigment as inorganic powder, and 30 g of hydrogenated polydecene as oil were added.
(실시예 10)(Example 10)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 소수성 색조안료 55g, 오일로 하이드로제네이티드폴리데센 30g, 첨가제로 폴리올인 다이프로필렌글리콜 5g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 55 g of hydrophobic color pigment as an inorganic powder, 30 g of oil-hydrogenated polydecene, and 5 g of dipropylene glycol, a polyol, were added as an additive. was manufactured.
(실시예 11)(Example 11)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 소수성 색조안료 35g, 합성플루오르플로고파이트 20g, 오일로 하이드로제네이티드폴리데센 30g, 첨가제로 폴리올인 다이프로필렌글리콜 5g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, 10 g of hydrophobic amorphous silica, 35 g of hydrophobic color pigment as inorganic powder, 20 g of synthetic fluorophlogopite, 30 g of oil-hydrogenated polydecene, and 5 g of dipropylene glycol, a polyol, as an additive were added. Microcapsules were prepared in the same manner as in 1.
(실시예 12)(Example 12)
분산액 제조 시, 소수성 무정형 실리카 10g, 무기분체로 기능성 분체인 합성플루오르플로고파이트 60g, 오일로 하이드로제네이티드폴리데센 30g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, microcapsules were prepared in the same manner as in Example 1, except that 10 g of hydrophobic amorphous silica, 60 g of synthetic fluorophlogopite, which is a functional powder as an inorganic powder, and 30 g of hydrogenated polydecene as an oil were added.
(비교예 1)(Comparative Example 1)
분산액 제조 시, 소수성 무정형 실리카 1g, 무기분체로 친수성 색조안료 70g, 오일로 하이드로제네이티드폴리데센 30g을 첨가한 것을 제외하고, 실시예 1과 동일한 방법으로 마이크로캡슐을 제조하였다.When preparing the dispersion, microcapsules were prepared in the same manner as in Example 1, except that 1 g of hydrophobic amorphous silica, 70 g of hydrophilic color pigment as inorganic powder, and 30 g of hydrogenated polydecene as oil were added.
실시예 1 내지 12 및 비교예 1의 방법으로 분산액 제조 시, 용매에 첨가하는 무정형 실리카, 무기분체, 오일, 지방산염 및 폴리올의 첨가량을 하기의 표 1에 나타내었다.When preparing the dispersion by the method of Examples 1 to 12 and Comparative Example 1, the amounts of amorphous silica, inorganic powder, oil, fatty acid salt, and polyol added to the solvent are shown in Table 1 below.
무정형실리카
(g)amorphous silica
(g) 		무기분체(g)Inorganic powder (g) 오일(g)Oil (g) 지방산염(g)Fatty salts (g) 폴리올
(g)polyol
(g)
친수성hydrophilic 소수성hydrophobic 친수성 색조안료Hydrophilic color pigment 소수성 색조안료Hydrophobic color pigment 기능성분체(합성플루오르플로고파이트)Functional ingredient (synthetic fluorophlogopite) 하이드로제네이티드폴리데센Hydrogenated polydecene 아이소노닐아니소노나노에이트Isononyl Anisononanoate 폴리하이드록시스테아릭애씨드Polyhydroxystearic acid 다이프로필렌글리콜Dipropylene glycol
실시예1Example 1 55 6565 3030
실시예2Example 2 1010 6060 3030
실시예3Example 3 1010 6060 3030
실시예4Example 4 1010 6060 3030
실시예5Example 5 1010 6060 1515 1515
실시예6Example 6 1010 3535 2525 3030
실시예7Example 7 1010 5959 3030 1One
실시예8Example 8 1010 4040 1919 3030 1One
실시예9Example 9 1010 6060 3030
실시예10Example 10 1010 5555 3030 55
실시예11Example 11 1010 3535 2020 3030 55
실시예12Example 12 1010 6060 3030
비교예1Comparative Example 1 1One 7070 3030
(실험예 1) 마이크로캡슐을 함유한 화장품의 관능평가(Experimental Example 1) Sensory evaluation of cosmetics containing microcapsules
상기 실시예 1 내지 12 및 비교예 1의 방법으로 제조한 마이크로캡슐을 수분 제형의 화장료에 첨가하여 화장품을 제조하였다. 실시예 1 내지 11 및 비교예 1은 색조 화장품이며, 실시예 12는 스킨케어 화장품으로 제조하였다. 화장품 연구 경력 3년 이상인 패널 10인을 대상으로 독특한 사용감, 밀착력, 발림성, 커버력 및 마무리감에 대한 관능평가를 실시하였다. 평가 결과는 하기의 표 2에 나타내었다.Cosmetics were manufactured by adding the microcapsules prepared by the methods of Examples 1 to 12 and Comparative Example 1 to water-based cosmetics. Examples 1 to 11 and Comparative Example 1 were color cosmetics, and Example 12 was manufactured as skin care cosmetics. Sensory evaluation of unique feeling of use, adhesion, spreadability, coverage, and finish was conducted on 10 panelists with more than 3 years of cosmetics research experience. The evaluation results are shown in Table 2 below.
독특한
사용감unique
feeling of use 		밀착력Adhesion 발림성Spreadability 커버력Coverage 마무리감sense of finish 총합total
실시예 1Example 1 44 33 44 33 44 3.63.6
실시예 2Example 2 44 33 44 33 44 3.63.6
실시예 3Example 3 33 22 44 33 44 3.23.2
실시예 4Example 4 44 1One 55 33 44 3.43.4
실시예 5Example 5 44 22 55 33 44 3.63.6
실시예 6Example 6 44 33 44 33 55 3.83.8
실시예 7Example 7 55 44 33 55 44 4.24.2
실시예 8Example 8 55 44 33 55 55 4.44.4
실시예 9Example 9 44 55 1One 55 33 3.63.6
실시예 10Example 10 55 44 33 55 44 4.24.2
실시예 11Example 11 55 44 33 55 55 4.44.4
실시예 12Example 12 33 -- 55 -- 55 4.34.3
비교예 1Comparative Example 1 22 22 33 22 33 2.42.4
1점 : 매우 나쁨, 2점 : 나쁨, 3점 : 보통, 4점 : 우수, 5점 : 매우 우수1 point: very bad, 2 points: bad, 3 points: average, 4 points: excellent, 5 points: very good
실시예 1 내지 12는 모두 비교예 1에 비해 우수한 성능을 가지고 있음을 확인할 수 있다. 그 중에서도 마이크로캡슐이 지방산염을 함유하는 실시예 7 내지 8과, 마이크로캡슐이 폴리올을 함유하는 실시예 10 내지 11의 관능평가 점수가 높은 것을 알 수 있다. 실시예 7 내지 실시예 8의 경우, 지방산염이 친수성 무기분체와 소수성 오일간의 불안정한 계면을 안정화하여 독특한 사용감을 확보하고, 화장품의 점도를 증가시켜 밀착력을 향상시킬 수 있다. 실시예 10 내지 실시예 11의 경우, 소수성 특성을 나타내는 무기분체가 친수성인 폴리올과 복합화되어, 수분 제형의 화장품에서도 이질감 없이 잘 섞일 수 있어, 사용자에게 사용감 및 밀착력을 향상시킬 수 있어 유리하다.It can be seen that Examples 1 to 12 all have superior performance compared to Comparative Example 1. Among them, it can be seen that Examples 7 to 8, in which microcapsules contain fatty acid salts, and Examples 10 to 11, in which microcapsules contain polyol, have high sensory evaluation scores. In the case of Examples 7 to 8, fatty acid salts can stabilize the unstable interface between the hydrophilic inorganic powder and the hydrophobic oil to ensure a unique feeling of use and increase the viscosity of the cosmetic to improve adhesion. In the case of Examples 10 and 11, the inorganic powder showing hydrophobic properties is complexed with the hydrophilic polyol, so that it can be mixed well without any discomfort even in water-based cosmetics, which is advantageous because it can improve the feeling of use and adhesion to the user.
(실험예 2) 마이크로캡슐의 표면 특성 평가(Experimental Example 2) Evaluation of surface properties of microcapsules
상기 실시예 2, 실시예 3, 실시예 7, 실시예 9, 실시예 10 및 비교예 1의 방법으로 제조한 마이크로캡슐의 SEM(모델명: CX-100S, 제조사: COXEM) 이미지를 도 1 내지 도 4에 나타내었다.SEM (model name: CX-100S, manufacturer: COXEM) images of the microcapsules prepared by the methods of Example 2, Example 3, Example 7, Example 9, Example 10, and Comparative Example 1 are shown in FIGS. It is shown in 4.
비교예 1의 경우를 제외하고, 실시예 2 내지 3, 실시예 7 및 실시예 9 내지 10은 높은 구형도를 갖는 마이크로캡슐을 형성하는 것을 확인할 수 있다.Except for Comparative Example 1, it can be confirmed that Examples 2 to 3, Example 7 and Examples 9 to 10 form microcapsules with high sphericity.
구체적으로, 도 1(a)는 실시예 2의 방법으로 제조된 마이크로캡슐의 SEM 이미지이고, 도 1(b)는 실시예 3의 방법으로 제조된 마이크로캡슐의 SEM 이미지이다. 도 1에 도시된 바와 같이, 쉘로 소수성 무정형 실리카를 포함하는 실시예 2 및 쉘로 친수성 무정형 실리카를 포함하는 실시예 3의 마이크로캡슐 모두 코어에 오일 및 무기분체를 고함량으로 포함함과 동시에 마이크로캡슐이 높은 구형도를 갖는 것을 확인할 수 있다.Specifically, Figure 1(a) is an SEM image of a microcapsule prepared by the method of Example 2, and Figure 1(b) is an SEM image of a microcapsule prepared by the method of Example 3. As shown in Figure 1, both the microcapsules of Example 2 containing hydrophobic amorphous silica as a shell and Example 3 containing hydrophilic amorphous silica as a shell contain a high content of oil and inorganic powder in the core, and at the same time, the microcapsules It can be confirmed that it has high sphericity.
도 2는 비교예 1에 따른 방법으로 제조된 마이크로캡슐의 SEM 이미지로, 무정형 실리카의 함유량이 적어 제조된 마이크로캡슐이 코어 물질을 충분히 감싸지 못해 구형의 마이크로캡슐이 형성되지 않고 캡슐이 깨져있는 형태인 것을 확인할 수 있다. Figure 2 is an SEM image of a microcapsule manufactured by the method according to Comparative Example 1. The microcapsule produced due to the low content of amorphous silica did not sufficiently surround the core material, so a spherical microcapsule was not formed and the capsule was broken. You can check that.
도 3은 실시예 7에 따른 방법으로 제조된 마이크로캡슐의 SEM 이미지를 도시한 도면이다. 도 3을 참조하면, 친수성 무기분체가 지방산염과 복합화되어 마이크로캡슐이 거친 표면을 형성한 것을 확인할 수 있다.Figure 3 is a diagram showing an SEM image of microcapsules manufactured by the method according to Example 7. Referring to Figure 3, it can be seen that the hydrophilic inorganic powder was complexed with the fatty acid salt to form a rough surface of the microcapsule.
도 4(a)는 실시예 9에 따른 방법으로 제조된 마이크로캡슐 및 도 4(b)는 실시예 10에 따라 제조된 마이크로캡슐의 SEM 이미지를 도시한 도면이다. 도 4에 도시된 바와 같이, 실시예 9 및 실시에 10의 경우, 무기분체로 소수성 색조 안료를 사용하여 마이크로캡슐의 표면이 거칠어진 것을 알 수 있다.Figure 4(a) shows a microcapsule prepared according to Example 9, and Figure 4(b) shows an SEM image of a microcapsule prepared according to Example 10. As shown in Figure 4, in Examples 9 and 10, it can be seen that the surface of the microcapsules was roughened by using a hydrophobic color pigment as an inorganic powder.
이상과 같이 본 발명에서는 특정된 사항들과 한정된 실시예 및 도면에 의해 설명되었으나 이는 본 발명의 보다 전반적인 이해를 돕기 위해서 제공된 것일 뿐, 본 발명은 상기의 실시예에 한정되는 것은 아니며, 본 발명이 속하는 분야에서 통상의 지식을 가진 자라면 이러한 기재로부터 다양한 수정 및 변형이 가능하다. As described above, the present invention has been described with specific details, limited embodiments, and drawings, but these are provided only to facilitate a more general understanding of the present invention, and the present invention is not limited to the above embodiments, and the present invention Anyone skilled in the art can make various modifications and variations from this description.
따라서, 본 발명의 사상은 설명된 실시예에 국한되어 정해져서는 아니되며, 후술하는 특허청구범위 뿐만 아니라 이 특허청구범위와 균등하거나 등가적 변형이 있는 모든 것들은 본 발명 사상의 범주에 속한다고 할 것이다.Accordingly, the spirit of the present invention should not be limited to the described embodiments, and the scope of the patent claims described below as well as all modifications that are equivalent or equivalent to the scope of this patent claim shall fall within the scope of the spirit of the present invention. .

Claims (15)

  1. 오일 및 무기분체를 함유하는 코어 및A core containing oil and inorganic powder and
    상기 코어 상에 위치하여 복수의 무정형 실리카 입자가 조밀하게 조립된 쉘을 포함하는 마이크로캡슐로서,A microcapsule including a shell in which a plurality of amorphous silica particles are densely assembled located on the core,
    상기 마이크로캡슐의 총 중량에 대해 80 내지 99 중량%의 오일 및 무기분체를 포함하고, 상기 쉘은 다공성을 가지는 것을 특징으로 하는 마이크로캡슐.A microcapsule comprising 80 to 99% by weight of oil and inorganic powder based on the total weight of the microcapsule, and the shell is porous.
  2. 제1항에 있어서,According to paragraph 1,
    상기 무정형 실리카 입자는 마이크로캡슐의 총 중량에 대해 1 내지 20 중량%를 포함하는 마이크로캡슐.A microcapsule containing 1 to 20% by weight of the amorphous silica particles based on the total weight of the microcapsule.
  3. 제1항에 있어서,According to paragraph 1,
    상기 무기분체의 중량이 상기 오일보다 더 많은 마이크로캡슐.Microcapsules in which the weight of the inorganic powder is greater than that of the oil.
  4. 제1항에 있어서,According to paragraph 1,
    상기 마이크로캡슐에 함유된 오일과 무기분체의 중량비는 1 : 1.5 내지 1 : 4인 마이크로캡슐.The weight ratio of oil and inorganic powder contained in the microcapsule is 1:1.5 to 1:4.
  5. 제1항에 있어서,According to paragraph 1,
    상기 무정형 실리카 입자의 평균입경(D50)은 400 내지 500nm인 마이크로캡슐.The average particle diameter (D 50 ) of the amorphous silica particles is a microcapsule of 400 to 500 nm.
  6. 제1항에 있어서,According to paragraph 1,
    상기 무정형 실리카 입자의 입도분포폭((D90-D10)/D50)은 0.9 내지 1.2인 마이크로캡슐.The particle size distribution width ((D 90 -D 10 )/D 50 ) of the amorphous silica particles is a microcapsule of 0.9 to 1.2.
  7. 제1항에 있어서,According to paragraph 1,
    상기 쉘은 200 내지 800 nm 입경의 기공을 포함하는 다공성 쉘인 마이크로캡슐. The shell is a microcapsule that is a porous shell containing pores with a particle diameter of 200 to 800 nm.
  8. 제1항에 있어서,According to paragraph 1,
    상기 마이크로캡슐의 평균입경은 30 내지 300 ㎛인, 마이크로캡슐.The microcapsule has an average particle diameter of 30 to 300 ㎛.
  9. 제1항에 있어서,According to paragraph 1,
    상기 무기분체는 지방산염과 복합화된 친수성 무기분체를 포함하는 마이크로캡슐.The inorganic powder is a microcapsule containing hydrophilic inorganic powder complexed with fatty acid salt.
  10. 제9항에 있어서,According to clause 9,
    상기 무기분체는 폴리올과 복합화된 소수성 무기분체를 포함하는 마이크로캡슐. The inorganic powder is a microcapsule containing hydrophobic inorganic powder complexed with polyol.
  11. 제1항에 있어서,According to paragraph 1,
    상기 무기분체는 이산화티탄, 산화철안료, 유기안료, 레이크염료, 천연안료, 합성플루오르플로고파이트, 산화아연, 질화붕소, 탈크, 카올린, 마이카, 견운모, 황산바륨, 판상알루미나, 펄 또는 이들의 혼합물을 포함하는 마이크로캡슐.The inorganic powder includes titanium dioxide, iron oxide pigment, organic pigment, lake dye, natural pigment, synthetic fluorophlogopite, zinc oxide, boron nitride, talc, kaolin, mica, sericite, barium sulfate, plate-shaped alumina, pearl, or mixtures thereof. Microcapsules containing.
  12. 제1항 내지 제11항 중 어느 한 항에 따른 마이크로캡슐을 함유하는 화장료 조성물.A cosmetic composition containing microcapsules according to any one of claims 1 to 11.
  13. 무정형 실리카 입자, 오일, 무기 분체 및 용매를 포함하는 분산액을 제조하는 단계; 및Preparing a dispersion containing amorphous silica particles, oil, inorganic powder, and solvent; and
    상기 분산액을 회전 분무 건조기로 분무 건조하여 마이크로캡슐 입자를 제조하는 단계;를 포함하며,It includes the step of spray drying the dispersion using a rotary spray dryer to produce microcapsule particles,
    상기 오일 및 무기분체는 상기 분산액의 총 중량에 대하여 10 내지 30 중량%를 함유하는, 마이크로캡슐의 제조방법.A method for producing microcapsules, wherein the oil and inorganic powder contain 10 to 30% by weight based on the total weight of the dispersion.
  14. 제13항에 있어서,According to clause 13,
    상기 마이크로캡슐 입자를 체분급기에 통과하여 선별하는 단계를 더 포함하는 마이크로캡슐의 제조방법.A method for producing microcapsules further comprising the step of passing the microcapsule particles through a sieve sorter to select them.
  15. 제13항에 있어서,According to clause 13,
    상기 용매는 에탄올 및 아세톤을 포함하는 군에서 선택되는 하나를 포함하는 마이크로캡슐의 제조방법.A method for producing microcapsules wherein the solvent includes one selected from the group consisting of ethanol and acetone.
PCT/KR2023/013408 2022-11-16 2023-09-07 Microcapsule containing high content of oil and amorphous silica, and method for producing same WO2024106708A1 (en)

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