WO2015088137A1 - 화장품용 조성물 - Google Patents
화장품용 조성물 Download PDFInfo
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- WO2015088137A1 WO2015088137A1 PCT/KR2014/010213 KR2014010213W WO2015088137A1 WO 2015088137 A1 WO2015088137 A1 WO 2015088137A1 KR 2014010213 W KR2014010213 W KR 2014010213W WO 2015088137 A1 WO2015088137 A1 WO 2015088137A1
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- pigment
- substrate
- natural
- cosmetic composition
- coating
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
-
- 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
- A61K8/0241—Containing particulates characterized by their shape and/or structure
- A61K8/0254—Platelets; Flakes
- A61K8/0258—Layered structure
- A61K8/0266—Characterized by the sequence of layers
-
- 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
- A61K8/29—Titanium; 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9794—Liliopsida [monocotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
- A61Q1/04—Preparations containing skin colorants, e.g. pigments for lips
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
- A61Q1/04—Preparations containing skin colorants, e.g. pigments for lips
- A61Q1/06—Lipsticks
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
- A61Q1/08—Preparations containing skin colorants, e.g. pigments for cheeks, e.g. rouge
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
- A61Q1/10—Preparations containing skin colorants, e.g. pigments for eyes, e.g. eyeliner, mascara
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q3/00—Manicure or pedicure preparations
- A61Q3/02—Nail coatings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/42—Colour properties
- A61K2800/43—Pigments; Dyes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/42—Colour properties
- A61K2800/43—Pigments; Dyes
- A61K2800/434—Luminescent, Fluorescent; Optical brighteners; Photosensitizers
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/42—Colour properties
- A61K2800/43—Pigments; Dyes
- A61K2800/436—Interference pigments, e.g. Iridescent, Pearlescent
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
- A61K2800/62—Coated
- A61K2800/621—Coated by inorganic compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/61—Surface treated
- A61K2800/62—Coated
- A61K2800/622—Coated by organic compounds
Definitions
- the present invention relates to a cosmetic manufacturing technology, and more particularly to a cosmetic composition comprising a vegetable natural pigment, a vegetable natural pigment coating gloss pigment, titanium oxide coating or iron oxide coating gloss pigment.
- Cosmetics are sensitive to changes in fashion, and various products are continuously released. Cosmetics include various components such as oils, pigments, and resins, and pigments of these elements determine the color of the cosmetics.
- Cosmetics are largely divided into base makeup products that are applied to the entire face and point makeup products that apply only a local part of the face.
- point makeup products include lipstick, eye shadow and blusher, and color is the most important factor in common.
- carmine which is an animal red pigment powdered by drying dried insects parasitic cactus.
- Carmine is widely used as a pigment that produces red color in cosmetics, drinks, and ice cream.
- Carmine can cause allergic reactions such as hives, rhinitis, and asthma in some people, and can cause hyperactivity disorder in children.
- Background art related to the present invention is a makeup composition containing a black color mixture of the pigment disclosed in the Republic of Korea Patent Publication No. 10-2012-0113661 (published October 15, 2012).
- An object of the present invention is to provide a cosmetic composition that can implement a variety of colors.
- Cosmetic composition according to an embodiment of the present invention for achieving the above object includes a pigment, a resin and a solvent, the pigment is a vegetable pigment, a vegetable pigment and a metallic pigment produced by coating a vegetable natural pigment on a substrate It characterized in that it can exhibit a variety of colors, including at least one of the pigments prepared by coating on the substrate.
- the pigment is preferably contained in 2 to 50% by weight of the total weight of the composition.
- the solvent is an oil
- the resin is an oil soluble resin
- the said cosmetic composition is for aqueous cosmetics
- the said solvent is water and the said resin is a water-soluble resin.
- the pigment may be a vegetable natural pigment or a bright pigment coated with a vegetable natural pigment on a substrate.
- the pigment is coated with a substrate of iron oxide, titanium dioxide or tin dioxide, it may be coated by a metal oxide coating reaction including the adsorption reaction and calcining.
- the cosmetic composition according to the present invention comprises at least one of red, yellow or blue glossy pigments prepared by coating a vegetable natural pigment, a vegetable natural pigment on a substrate and a metal oxide coated on a substrate. Including, it may represent red, yellow and blue, as well as a variety of colors, such as green, purple, pink, purple, black, white, gray through a mixture of pigments.
- Cosmetic composition according to an embodiment of the present invention is mascara, eye shadow, liquid eyeliner, gel eyeliner, nail enamel, foundation, lipstick, lip gloss, cosmetic cream, makeup foundation, eye pencil, blusher or emulsion, etc.
- pigments, resins and solvents are included in the same manner as in general cosmetic compositions.
- the pigment is one or more of red, yellow or blue glossy pigments prepared by coating a vegetable natural pigment, a vegetable natural pigment on the substrate and a red, yellow or blue glossy pigment and a metal oxide coated on the substrate.
- Including a red, yellow, blue can be represented as well as a variety of colors, such as green, purple, pink, purple, black, white, gray through a mixture of pigments representing different colors.
- the pigment when using a natural pigment, may be a natural pigment itself or a coating of a natural pigment containing a vegetable natural dye on the substrate.
- the pigment when using a metal oxide, is coated with a substrate of iron oxide, titanium dioxide or tin dioxide, it may be coated by a metal oxide coating reaction including the adsorption reaction and sintering.
- the pigment is preferably contained in 2 to 50% by weight of the total weight of the composition. If the content of the pigment is less than 2% by weight, it may be difficult to sufficiently express the desired color. On the contrary, when the content of the pigment exceeds 50% by weight, there is a problem in that the aggregation of the pigment occurs excessively, or the shelf life is lowered.
- the cosmetic composition according to the present invention may be for oily cosmetics or for aqueous cosmetics, and more preferably for oily cosmetics.
- the solvent may be an oil
- the resin may be an oil soluble resin.
- oil-soluble resins may be represented by ethyl cellulose, propyl cellulose, vinyl ester copolymers, and the like, and various oil-soluble resins used for manufacturing cosmetics may be used.
- the solvent may be water
- the resin may be a water-soluble resin.
- a water-soluble resin may be protein, keratin, polyacrylate or polymethacrylate, polyvinylpyrrolidone, polyvinyl alcohol and the like, and various other known water-soluble resins may be used.
- the solvent may include about 10 to 40% by weight in the case of solid cosmetics, and may include about 50 to 80% by weight in the case of liquid cosmetics, but is not limited thereto. Additional procedures may be included.
- the cosmetic composition according to the present invention may further include various additives such as a moisturizer or a humidifier, an anti-aging agent, and an antimicrobial agent.
- Examples of the method of manufacturing a gloss pigment using a natural pigment include preparing a primary pigment (natural pigment) by titrating an inorganic salt solution to a vegetable natural dye, and then adjusting the pH to 5 to 7, and adjusting the acidity to the substrate suspension. Mixing the primary pigment to form an oxide layer on the surface of the substrate to produce a gloss pigment. This method is more suitable when using red, yellow, purple, green or black natural dyes.
- the method for producing a gloss pigment is a step of obtaining a natural dye from a dye, preparing a pigment from a natural dye, by titrating an inorganic salt solution to the dye, a primary pigment (natural pigment) comprising a natural dye Forming, synthetic mica, natural mica, glass flake (plate glass), plate iron oxide, plate alumina and plate silica, talc, bismuth, including a flake substrate and metal oxide coated gloss pigment composition water Forming a substrate suspension which is mixed with ionized water, distilled water, and the like, followed by stirring and dispersing; and coating a flake substrate by mixing an acidity regulator and the pigment with the substrate suspension to coat an oxide layer on the surface of the flake substrate.
- the primary pigment (natural pigment) manufacturing step a dye manufacturing step of producing a dye from a natural salt material, a dye metal salt mixed solution preparation step of adding a dye to a metal salt-containing solution, the step of stirring the dye metal salt mixed solution, the dye metal salt Pigment particle immersion step of immersing the pigment particles in the mixed solution and the pigment particle drying step of separating and drying the immersed pigment particles.
- the salt solution extraction step of extracting the salt solution by adding and heating 10 to 30 parts by weight of the natural dye and the salt solution drying step of concentrating and vacuum drying the extracted salt solution Include.
- the natural dye may be a red, yellow, purple, blue, green or black natural dyes.
- the dyeing of the natural dye is madder (safflower), safflower (safflower), joiner (sappanwood), logwood (logm), persimmon (gromwell), persimmon (persimmon), apricot, plum, gingko, ginger, Red or purple, at least any one selected from precipitation roots, cucurbita, kojang-geun, hiking tree, yew, Schisandra chinensis, camellia, grape, iris, and combinations thereof, gardenia, turmeric, onion peel, safflower yellow cattle, Yellow or green series, at least one selected from rhubarb, yellowish white, cloves, pomegranate, reeds, lumps, ash, lacquer, spruce, red bean, forsythia bark, larva, alder, chestnut, oak and combinations thereof Can be.
- the inorganic salt may be a metal salt
- the metal salt may be BaCl 2 , CaCl 2 , AlCl 3 , SnCl 4 , TiCl 4 , TiOCl 2 , TiOSO 4 , FeCl 3 , FeSO 4 , SiCl 4, ZrOCl 2
- the dye metal salt mixed solution may be prepared to include an integer of 100 parts by weight, 3 parts by weight to 30 parts by weight of the dye and 3 parts by weight to 30 parts by weight of the metal salt.
- the dye metal salt mixed solution is stirred.
- the dye metal salt mixed solution was heated to 200 rpm to 300 rpm at 20 ° C. to 60 ° C. and stirred, and the NaOH, KOH, Ca (OH) 2 , NH 3 , Mg (OH) 2 , and CH 3 NH 2 were added to the dye metal salt mixed solution.
- CH 3 CH 2 NH 2 , CH 3 OH, Al (OH) 3 A basic solution comprising one or more selected mixtures is added to adjust the pH to 5 to 7 to soak the pigment particles. In the temperature range below 20 ° C, the efficiency of the reaction is lowered, and in the temperature range above 60 ° C, the color of the pigment may change.
- the dipped pigment particles are separated and dried.
- the pigment forming step includes a pigment milling step of milling the pigment and a pigment dispersion step of mixing and stirring and dispersing the pigment in purified water.
- the pigment is preferably sufficiently milled for 12 to 24 hours at 200rpm to 500rpm.
- the volume of milling balls in a 500 mL container is 300 mL. If the volume of the milling ball is less than 300 mL, the efficiency of milling is reduced and the dispersion of aggregated pigment particles is uneven. Degrades. Milling from a minimum of 12 hours up to a maximum of 24 hours. When milling below 200 rpm, the effect of dispersion decreases. When milling above 500 rpm, the dispersion effect does not increase any more, and when it exceeds 500 rpm, the pigment particles may be damaged. It is important to improve the dispersion of the pigment particles.
- the primary pigment (natural pigment) can be prepared by the above process.
- a mixture of a flake substrate and a metal oxide-coated pigment composition comprising at least one of synthetic mica, natural mica, Glass Flake, plate iron oxide, plate alumina and plate silica, talc, and bismuth is mixed with DI water.
- the substrate suspension forming step of stirring and dispersing may be performed at 200 rpm to 500 rpm.
- the acidity regulator and the pigment are mixed with the substrate suspension formed in the substrate suspension forming step to coat the surface of the flake substrate with pigment particles containing a vegetable natural dye component.
- the acidity regulator may use an acidic solution containing one or more mixtures selected from hydrochloric acid, sulfuric acid, acetic acid, acetic acid, and the like, indicating acidity.
- the coating reaction is adjusted to a pH of 4.0 to 8.0 of the mixed solution of the substrate suspension and the pigment, it is preferably carried out for 30 to 60 minutes at 200rpm to 500rpm.
- a flake substrate drying step of drying the washed flake substrate and a flake substrate formed larger than a predetermined size of the dried flake substrate After the flake substrate coating step, washing and dehydrating the flake substrate coated with an oxide layer, a flake substrate drying step of drying the washed flake substrate and a flake substrate formed larger than a predetermined size of the dried flake substrate.
- the flake substrate screening step of separating using a mesh is further included.
- the flake substrate drying step may be carried out at 60 °C to 100 °C for 12 hours to 24 hours.
- the flake substrate to be separated is 45 ⁇ m or less.
- a mesh may be used to remove aggregated particles generated during the reaction.
- Another example of the method of manufacturing a natural pigment using a gloss pigment after preparing a primary pigment from a vegetable natural salt, to produce a natural pigment by ball milling, adding a substrate and a primary pigment in water, and then stirring and Titrating and stirring the inorganic salt solution to the stirred result, thereby forming an oxide layer on the surface of the substrate.
- This method is preferred when using mainly blue or green dyes.
- the natural pigment manufacturing method includes a step of obtaining a natural dye from the dye, a pigment manufacturing step of producing a pigment from a blue-based natural dye, a ball milling step of adding water to the pigment and ball milling.
- a method of manufacturing a gloss pigment coated with a natural pigment on the substrate is a flake substrate and a metal oxide including one or more of synthetic mica, natural mica, Glass Flake (plate glass), plate iron oxide, plate alumina and plate silica, talc, bismuth
- Pigment production step when 100 parts by weight of distilled water or organic solvent, 5 to 30 parts by weight of the natural dye is added to the salt extraction step of extracting the salt solution by heating and the salt solution drying step of concentrating and vacuum drying the extracted salt solution Include.
- the natural dye may be a blue or green natural dyes.
- the salt of the natural dye may be a blue or green series of at least one selected from indigo, chicken fowl, iris and combinations thereof.
- the pigment when the integer is 100 parts by weight, the pigment is preferably contained in 10 parts by weight to 30 parts by weight.
- the reaction efficiency may be lowered due to the low concentration, and when the pigment is more than 30 parts by weight, the reaction efficiency may be lowered because the amount of the natural pigment is too large relative to the reaction solution.
- ball milling is preferably performed for 6 hours to 12 hours. If the ball milling time is less than 6 hours, the dispersion may be insufficient, and if the ball milling time is longer than 12 hours, the efficiency may be reduced due to the long process time without further dispersing effect.
- Natural pigment can be prepared through the above process.
- the substrate In the step of forming the substrate suspension, the substrate has an average particle diameter of 2 to 250 ⁇ m and a thickness of 0.2 to 5 ⁇ m.
- the average particle diameter is less than 2 ⁇ m, the same color with constant refractive index may not be exhibited due to scattering of light due to the reduction of the angular ratio. Formation of the oxide layer can be difficult.
- the substrate suspension when the substrate suspension is 100 parts by weight, the substrate is preferably contained in 3 to 15 parts by weight. If the concentration of the substrate is less than 3 parts by weight, the concentration may be too low to reduce the reaction efficiency, and if more than 15 parts by weight, aggregation may occur due to the thick concentration.
- the stirring is carried out at room temperature, the stirring speed is preferably 200rpm to 500rpm. If the stirring speed is less than 200rpm, the dispersion effect during the reaction may be agglomerated between the pigments, and if it exceeds 500rpm can be reduced efficiency only by increasing the rpm without further dispersion effect.
- the inorganic salt solution is titrated and stirred to adjust the pH of the substrate suspension to coat an oxide layer on the surface of the flake substrate.
- the substrate may be a flake substrate including one or more of synthetic mica, natural mica, Glass Flake (plate glass), plate iron oxide, plate alumina and plate silica, talc, bismuth or may be coated with a metal oxide.
- the pH may be adjusted in at least two pH adjustment steps.
- the pH adjustment step the first pH adjustment step of adjusting the pH to 7 ⁇ 7.1 by slowly titrating a metal salt solution of 3 to 10% by volume in the substrate suspension and stirring for 5 to 30 minutes, the concentration of 3 to 10% by volume
- the second pH adjustment step of slowly titrating the metal salt solution and stirring for 5-30 minutes to adjust the pH to 4 to 4.1, gradually titrating the HCl solution of 10-20% by volume and stirring for 5-30 minutes to adjust the pH.
- a flake substrate drying step of drying the washed flake substrate and a flake substrate formed larger than a predetermined size of the dried flake substrate After the flake substrate coating step, washing and dehydrating the flake substrate coated with an oxide layer, a flake substrate drying step of drying the washed flake substrate and a flake substrate formed larger than a predetermined size of the dried flake substrate.
- the flake substrate screening step of separating using a mesh is further included.
- the flake substrate drying step may be carried out at 60 °C to 100 °C for 6 hours to 12 hours.
- the flake substrate to be separated is 45 ⁇ m or less.
- a mesh may be used to remove aggregated particles generated during the reaction.
- the red pigment may be prepared by coating iron oxide (Fe 2 O 3 ) as a metal oxide.
- the specific manufacturing process is as follows.
- a plate-like substrate containing at least one of natural mica, synthetic mica, flaky alumina, glass flake, plate iron oxide, plate silica, talc and bismuth is watered.
- the suspension is suspended in demineralized water and stirred using a stirrer to prepare a slurry.
- the slurry production for the pigment production it is preferable to heat the slurry to increase the temperature of the slurry to 60 ⁇ 90 °C.
- the reason for heating the slurry is that when the temperature of the slurry is less than 60 ° C., the coating state of the subsequent coating layer is not uniform, and the size and shape of the material to be coated become very irregular. This is because when the temperature of the slurry exceeds 90 ° C., the reaction for coating may occur violently to form a rough coating layer. Since the pigment does not have high saturation when the state of the coating layer coated on the substrate is unstable, it is preferable to maintain the above temperature range.
- the pH of the slurry it is preferable to adjust the pH of the slurry to 2.5 to 4.0 so that FeCl 3 can be hydrolyzed by adding an acid, for example, hydrochloric acid (HCl) solution, to the slurry.
- an acid for example, hydrochloric acid (HCl) solution
- Lower Fe 2 O 3 layer coating step is FeCl 3 solution to a slurry, elevated temperatures, when completing the pH adjustment, followed by a lower Fe 2 O 3 layer is from 10 to 30% by weight of the slurry in the coating step, the solution within the FeCl 3 content Weigh and add titrate.
- the pH of a slurry is kept constant at 2.5-4.0 by adding the base, for example, the sodium hydroxide (NaOH) aqueous solution diluted to 10-50%.
- the FeCl 3 content is less than 10% by weight, the amount of production that can be produced at a time during manufacture is reduced, the productivity is significantly reduced. On the other hand, if it exceeds 30% by weight, the reactivity is generally poor, the surface is not smooth, and impurities are increased.
- the Fe 2 O 3 layer is coated on the surface of the small plate substrate by hydrolyzing FeCl 3 chloride (metal salt) in the FeCl 3 solution in an aqueous medium. At this time, the Fe 2 O 3 layer becomes a lower Fe 2 O 3 layer.
- the MgO.SiO 2 solution is weighed and titrated into a slurry including a lower Fe 2 O 3 layer so that the MgO.SiO 2 content in the solution becomes 2 to 20% by weight.
- an acid for example, a hydrochloric acid solution is added to keep the pH of the slurry constant at 5-9.
- an acid for example, a hydrochloric acid solution is added to adjust the pH of the slurry to 2.5 to 4.0, and stirred for about 10 minutes to 1 hour to reflux.
- the MgO.SiO 2 content is less than 2% by weight, the amount of production that can be produced at a time during manufacture is reduced, resulting in a significant drop in productivity.
- the MgO.SiO 2 content exceeds 20% by weight, the reactivity is generally low, the surface is not smooth, and impurities are increased.
- the pH value of the slurry is out of the above range, the coating of the MgO.SiO 2 layer is not normally made or the coating material is not uniform and has an irregular size and shape, so that the pigment may not have a high saturation.
- the MgO.SiO 2 layer is coated on the surface of the lower Fe 2 O 3 layer by hydrolysis of the MgO.SiO 2 chloride in the MgO.SiO 2 solution in an aqueous medium.
- the upper Fe 2 O 3 layer coating step is titrated by adding a FeCl 3 solution to a slurry containing MgO.SiO 2 layer so that the FeCl 3 content in the solution is 10 to 30% by weight.
- a salt for example, an aqueous sodium hydroxide (NaOH) solution diluted to 10-50% is added to maintain the pH of the slurry at 2.5-4.0 and stirred for about 10 minutes to 1 hour to reflux.
- This upper Fe 2 O 3 layer coating process is performed in the same manner as the lower Fe 2 O 3 layer coating process described above.
- the Fe 2 O 3 layer is coated on the surface of the MgO.SiO 2 layer by hydrolysis of the FeCl 3 chloride in the FeCl 3 solution in an aqueous medium. At this time, the Fe 2 O 3 layer becomes an upper Fe 2 O 3 layer.
- each coating layer It is preferable to stabilize the state of each coating layer by maintaining the temperature of the slurry heated at the slurry manufacturing step from the lower Fe 2 O 3 layer coating step to the upper Fe 2 O 3 layer coating step.
- the coating thickness of the metal oxide increases according to the coating of the titrant, and the color appears in the order of Bronze, Orange, Copper, Red, and Bluish Red depending on the thickness.
- the reaction is stopped at the desired color. In particular, it is advantageous to stop the reaction in this color because of its high saturation in red.
- the slurry is stirred for about 10 minutes to 1 hour, the final slurry is filtered and dehydrated, washed several times with demineralized water, and then dried at 80 to 150 ° C. for about 1 to 20 hours to obtain a residue.
- Intermediates can be obtained.
- the calcination step calcinates the intermediate, the residue obtained from the final slurry, at a temperature of 600-900 ° C. to complete the synthesis of the pigment. At this time, if the calcination temperature is less than 600 °C, calcination is insufficient to obtain the desired pigment, if it exceeds 900 °C the substrate can reach the melting point and melt, producing a product other than the pigment to be obtained.
- the resulting final pigments are formed by coating the metal oxide layer on the surface of the Fe 2 O 3 / MgO ⁇ SiO 2 / Fe 2 O 3 stacked structure of small plate-shaped base material.
- the pigments according to the present invention can be easily wet-chemically produced by hydrolysis of metal salts in an aqueous medium, making the manufacturing process simple and economical.
- the method for producing a yellow pigment coated with a metal oxide on glass flakes is as follows.
- glass flakes for example, 5 ⁇ m thick glass substrate
- the glass flakes have a range of about 5 to 20% by weight.
- deionized water to prevent adsorption by ions.
- the reaction temperature of the dispersion of the glass flake particles is suitably 60 ⁇ 80 °C.
- the precursor material of tin dioxide is SnCl 2
- the precursor material of titanium dioxide is TiCl 4 (TiOCl 2 dissolved in an aqueous solution), TiOSO 4, and the like.
- the pH of the dispersion is maintained at an appropriate level, preferably 1.5 to 3 during the addition of the precursor material.
- hydrochloric acid is added to make pH 1.5 to 3, and then tin hydroxide hydrated on the substrate according to the precursor of metal oxide. Is adsorbed first and hydrated titanium dioxide is adsorbed.
- a basic aqueous solution such as sodium hydroxide is simultaneously added to adsorb the hydrated metal oxide. It is important to titrate the precursor material of the metal oxide while maintaining the pH range in the process.
- the firing temperature for forming the metal oxide after the reaction is preferably 400 ⁇ 600 °C. It has a process of removing aggregated particles generated during the reaction through screening after firing.
- Pigment coated with a metal oxide on the glass flakes prepared by the above process has a high gloss due to the size of the particles and a strong sparkling effect due to the thickness.
- the manufacturing method of the blue or purple luster pigment coated with the metal oxide on the synthetic mica particles is as follows.
- the synthetic mica particles are dispersed in water, wherein the particles are preferably in the range of about 5 to 15% by weight. At this time, it is preferable to use deionized water in order to prevent adsorption interference by ions.
- the precursor material of metal oxide, or a mixture thereof is added to the said dispersion liquid,
- the precursor component of this metal oxide coated in this invention is a precursor of tin dioxide.
- the material include SnCl 2
- precursor materials of the titanium dioxide include TiCl 4 (TiOCl 2 dissolved in an aqueous solution), TiOSO 4, and the like.
- the pH of the dispersion is maintained at an appropriate level, preferably 1 to 4 during the addition of the precursor material.
- the acid preferably hydrochloric acid, is added to pH 1 to 4, and then the precursor of the metal oxide is added to the substrate phase.
- Hydrated tin dioxide is first adsorbed to the hydrated titanium dioxide. At this time, a basic aqueous solution such as sodium hydroxide is simultaneously added to adsorb the hydrated metal oxide. It is important to titrate the precursor material of the metal oxide while maintaining the pH range in the process.
- the metal oxide coating layer may be formed in a rutile crystal structure.
- the coating thickness of the hydrated metal oxide increases with titration to the dispersion of the precursor material, and the color appears in the order of silver, yellow, red, blue, and green according to the thickness. Stop the reaction. In particular, it is advantageous to stop the reaction in both colors because it will show high saturation in purple and blue.
- the synthetic mica coated as described above is commercialized through filtration, washing, drying, and calcining steps, and finally mass-produced through a screening step. The process after the coating step is easily accomplished by methods already known in the art.
- joiner's pigment 140 parts by weight of purified water and 60 parts by weight of joiner's pigment are added to a beaker of 500 mL, and milling is carried out at 70 rpm for 12 hours to form joiner's pigment .
- Potassium hydroxide was added to the joiner pigment to adjust the pH to 11.
- the pH of the mixed solution was adjusted to 5 again by adding a substrate suspension, a joiner pigment and CaCl 2 to a 2 L beaker.
- red joiner natural pigment After coating the red joiner natural pigment, it was washed with water and dewatered, and dried at 80 ° C. to produce a red gloss pigment coated with a red joiner pigment.
- screening was performed using a 325 mesh sieve to remove aggregated particles generated during the reaction.
- the natural dye extracted from Gardenia which is a natural dye salt
- purified water or an organic solvent
- purified water or an organic solvent
- vacuum drying to prepare a dye.
- 20 parts by weight of Gardenia dye was placed in a 2L beaker, and 100 parts by weight of purified water and 30 parts by weight of AlCl 3 were added and stirred at 200 rpm.
- the reaction temperature is set to 60 °C and sodium hydroxide is added.
- the pH is adjusted to 7 and the precipitate begins to form while stirring the solution, it is dehydrated, dried and ground to use as a pigment.
- Potassium hydroxide was added to the gardenia pigment to adjust the pH to 11.
- the pH of the mixed solution was adjusted to 5 again by adding a substrate suspension, gardenia pigment and CaCl 2 to a 2 L beaker.
- screening was performed using a 325 mesh sieve to remove aggregated particles generated during the reaction.
- the natural dye extracted from Cheongdae which is a salt of natural dyes, is heated in purified water (or an organic solvent) to concentrate the extracted salt solution, followed by vacuum drying to prepare a pigment. 20 parts by weight of blue pigment was added to a 250 ml ball milling bottle, and 80 parts by weight of purified water was added thereto, followed by ball milling for 6 hours.
- the pH was adjusted to 7.0 by slowly titrating a 5% by volume AlCl 3 solution to the substrate suspension and stirring for 10 minutes.
- the pH was then adjusted to 4.0 by slowly titrating a 5% by volume CaCl 2 solution and stirring for 10 minutes.
- the pH was then adjusted to 2.2 by titration of 15 vol% HCl solution slowly and stirring for 30 min.
- the pH was adjusted to 4.3 by slowly titrating 15 vol% KOH solution and stirring for 30 minutes.
- screening was performed using a 325 mesh sieve to remove aggregated particles generated during the reaction.
- FeCl 3 solution FeCl 3 content 20.0% by weight
- 600 g of FeCl 3 solution FeCl 3 content 20.0% by weight
- titration reflux for 10 minutes and adjust to pH 6.8 with dilution 10-30% NaOH.
- FeCl 3 solution FeCl 3 content 20.0 wt% was weighed and added to the slurry, followed by titration at a constant rate over about 5 hours while maintaining a constant pH of 3.5 with a 10-50% NaOH diluent. After titration, the mixture was stirred and refluxed for an additional 30 minutes. After refluxing, the mixture was adjusted to pH 8.0-8.5 with a dilution solution of 10-30% NaOH, refluxed for 30 minutes, stirred, and then the final slurry was filtered and dehydrated by washing, washed twice with demineralized water, and washed at 120 ° C for 10 minutes. Drying over time gave an intermediate, a residue in the form of a powder.
- the mixture was stirred for 30 minutes, and then titrated with 100 ml of 20% concentration of TiCl 4 solution, and the pH was maintained at 1.9 with 20% concentration of NaOH.
- synthetic mica was ground and classified to obtain synthetic mica particles having an average particle size of 12 ⁇ m, respectively. After adding 100 parts by weight of the synthetic mica particles, purified water was added to a total of 1000 parts by weight and dispersed at 300 rpm to form a substrate suspension. Thereafter, heating was performed up to 80 ° C.
- the mixture was stirred for 30 minutes, and then titrated with 120 mL of 40% concentration of TiOCl 2 solution, and the pH was maintained at 2.2 with 20% concentration of NaOH.
- the mixture was refluxed for 10 minutes, and the pH was adjusted to 8 using 20% NaOH aqueous solution. Then, after adjusting the pH to 1.7 with 10% aqueous HCl solution, SnCl 2 and TiOCl 2 aqueous solution were added in the same condition as above, and the color change appeared in the order of yellow, red, purple, and blue according to the thickness of titanium dioxide. Stop the reaction in blue while observing that.
- the mixture was stirred for 30 minutes, washed twice with water and then dried at 100 ° C. for 2 hours. After firing at 800 ° C. in an electric furnace, a blue pigment having high saturation was obtained, and then screened using a 325 mesh sieve to remove aggregated particles generated during the reaction.
- Glossy pigment prepared according to an embodiment of the present invention may be utilized as a pigment of cosmetics, such as mascara, eye shadow, eyeliner (liquid, gel), nail enamel and the like.
- [Table 1] to [Table 5] shows the composition of mascara, eye shadow, liquid eyeliner, gel eyeliner and nail enamel comprising a pigment prepared according to the embodiment.
- Table 1 shows the composition of mascara to which the pigment prepared according to the example is applied.
- Table 2 shows the composition of the eye shadow to which the pigment prepared according to Example 2 is applied.
- Table 3 shows the composition of the liquid eye shadow to which the pigment prepared according to Example 3 is applied.
- Table 4 shows the composition of the gel eyeshadow to which the pigment prepared according to Example 4 is applied.
- Table 5 shows the composition of the nail enamel to which the pigment prepared according to Example 1 is applied.
- [Table 6] is a sensory evaluation (0 ⁇ 100 points), such as the feeling of use as cosmetics for 40 women paneling from 20 to 40 to evaluate the applicability, hiding power, color and matte feeling of each product Scores, and the average value belongs to the evaluation.
- the pigment prepared according to the example when used as a cosmetic pigment, it exhibits application property, hiding power, transparency and excellent color. This means that, in the case of the gloss pigment according to the present invention, it can maintain a function equal to or higher than that of a conventionally used cosmetic pigment.
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Abstract
Description
Claims (8)
- 안료, 수지 및 용제를 포함하고,상기 안료는 천연안료, 천연안료를 기질에 코팅하여 제조한 광택 안료 및 금속산화물을 기질에 코팅하여 제조한 광택 안료 중 1종 이상을 포함하여 다양한 색상을 나타낼 수 있는 것을 특징으로 하는 화장품용 조성물.
- 제1항에 있어서,상기 안료는 조성물 전체 중량의 2~50중량%로 포함되는 것을 특징으로 하는 화장품용 조성물.
- 제1항에 있어서,상기 화장품용 조성물이 유성 화장품용인 경우,상기 용제는 오일이고, 상기 수지는 유용성(oil soluble) 수지인 것을 특징으로 하는 화장품용 조성물.
- 제1항에 있어서,상기 화장품용 조성물이 수성 화장품용인 경우,상기 용제는 물이고, 상기 수지는 수용성 수지인 것을 특징으로 하는 화장품용 조성물.
- 제1항에 있어서,상기 안료는 식물성 천연염료를 함유하는 천연안료이거나, 식물성 천연염료를 함유하는 천연안료를 기질에 코팅한 광택 안료인 것을 특징으로 하는 화장품용 조성물.
- 제1항에 있어서,상기 안료는 금속산화물을 기질에 코팅한 것으로, 흡착반응 및 소성을 포함하는 금속산화물 코팅 반응으로 코팅한 것을 특징으로 하는 화장품용 조성물.
- 제6항에 있어서,상기 금속산화물은 산화철, 이산화티탄 및 이산화주석 중 1종 이상을 포함하는 것을 특징으로 하는 화장품용 조성물.
- 제1항에 있어서,상기 화장품은 마스카라, 아이쉐도우, 액상 아이라이너, 젤상 아이라이너, 네일 에나멜, 파운데이션, 립스틱, 립글로스, 화장용 크림, 메이크업 파운데이션, 아이펜슬, 블러셔 또는 에멀젼인 것을 특징으로 하는 화장품용 조성물.
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EP14870326.7A EP3081210B1 (en) | 2013-12-13 | 2014-10-28 | Cosmetic composition |
JP2016539143A JP2016540018A (ja) | 2013-12-13 | 2014-10-28 | 化粧品用組成物 |
CN201480068057.3A CN105813629B (zh) | 2013-12-13 | 2014-10-28 | 化妆品用组合物 |
US15/104,145 US10285918B2 (en) | 2013-12-13 | 2014-10-28 | Cosmetic composition |
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KR1020130155675A KR101942912B1 (ko) | 2013-12-13 | 2013-12-13 | 화장품용 조성물 |
KR10-2013-0155675 | 2013-12-13 |
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EP (1) | EP3081210B1 (ko) |
JP (1) | JP2016540018A (ko) |
KR (1) | KR101942912B1 (ko) |
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RU2644178C1 (ru) * | 2016-11-24 | 2018-02-08 | Федеральное государственное автономное образовательное учреждение высшего образования "Белгородский государственный национальный исследовательский университет" (НИУ "БелГУ") | Способ получения пигментов для натуральных красок |
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KR102211786B1 (ko) | 2019-01-03 | 2021-02-04 | 씨큐브 주식회사 | 흡수성 및 흡유성이 향상된 화장품용 조성물 |
CN110200852B (zh) * | 2019-06-06 | 2022-05-20 | 广州微肽生物科技有限公司 | 一种光智能底妆产品及其制备方法 |
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US10285918B2 (en) | 2019-05-14 |
US20160361241A1 (en) | 2016-12-15 |
CN105813629A (zh) | 2016-07-27 |
JP2016540018A (ja) | 2016-12-22 |
EP3081210B1 (en) | 2019-06-12 |
KR20150069363A (ko) | 2015-06-23 |
CN105813629B (zh) | 2019-06-18 |
KR101942912B1 (ko) | 2019-01-28 |
EP3081210A4 (en) | 2017-05-31 |
EP3081210A1 (en) | 2016-10-19 |
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