WO2020111359A1 - Method for preparing wrinkle-shaped polymethylsilsesquioxane particles, and polymethylsilsesquioxane powder comprising polymethylsilsesquioxane particles prepared thereby - Google Patents

Method for preparing wrinkle-shaped polymethylsilsesquioxane particles, and polymethylsilsesquioxane powder comprising polymethylsilsesquioxane particles prepared thereby Download PDF

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WO2020111359A1
WO2020111359A1 PCT/KR2018/015306 KR2018015306W WO2020111359A1 WO 2020111359 A1 WO2020111359 A1 WO 2020111359A1 KR 2018015306 W KR2018015306 W KR 2018015306W WO 2020111359 A1 WO2020111359 A1 WO 2020111359A1
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pmsq
particles
corrugated
manufacturing
polymethylsilsesquioxane
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PCT/KR2018/015306
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French (fr)
Korean (ko)
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이영철
오승식
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이영철
(주) 우석켐
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
    • 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
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/12—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing organo-metallic compounds or metal hydrides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/06—Preparatory processes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/06—Preparatory processes
    • C08G77/08—Preparatory processes characterised by the catalysts used
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/26—Optical properties

Definitions

  • the present invention relates to a method for producing corrugated polymethylsilsesquioxane particles and a polymethylsilsesquioxane powder comprising polymethylsilsesquioxane particles produced therefrom.
  • Cosmetics to improve wrinkles can be divided into functional cosmetics that basically remove wrinkles by acting on factors that cause wrinkles, and cosmetics that have temporary concealing effect by filling the wrinkles with light and diffused light from the wrinkles. .
  • the principle of diffuse reflection of light is as follows.
  • light is irradiated to a material
  • part of the light is reflected from the surface, and part of it is transmitted.
  • light is refracted at a specific angle and transmitted according to the refractive index of the material.
  • a part of the light is reflected from the particles located on the surface and the rest is refracted at a specific angle and transmitted.
  • the transmitted light has the same phenomenon on the surface of the second particle inside.
  • the light reflected from the surface of the second particle is reflected at a different angle from the light reflected from the first particle. .
  • this phenomenon occurs continuously between the particles located inside, the reflected lights are reflected at different angles, and finally the light is diffusely reflected.
  • the present invention is to solve the above-mentioned problems, the object of the present invention is to provide a wrinkle-like polymethylsilsesquioxane particles having excellent skin texture with excellent embossing effect and excellent diffuse reflection properties, and a method for manufacturing the same.
  • a method of manufacturing corrugated PMSQ particles comprises: preparing a catalyst solution by mixing a selected catalyst with an organic solvent; Preparing a reaction solution by adding two or more different silanes to the catalyst solution; And synthesizing PMSQ (polymethylsilsesquioxane) particles having wrinkles on the surface through the reaction solution.
  • PMSQ polymethylsilsesquioxane
  • the two or more different types of silanes methyltriethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, dimethyldiethoxysilane, normal propyl Trimethoxysilane (N-propyltrimethoxysilane), N-propyltriethoxysilane, Vinyltrimethoxysilane, Vinyltriethoxysilane, Phenyltrimethoxysilane, It may include at least two selected from the group consisting of phenyltriethoxysilane, diphenyldimethoxysilane and methylphenyldimethoxysilane.
  • the two or more different types of silanes are methyltriethoxysilane and methyltrimethoxysilane, and the addition ratio of the methyltriethoxysilane and the methyltrimethoxysilane is It may be 4:1 (mole) to 1:4 (mole).
  • the higher the addition ratio of the methyl trimethoxysilane, the higher the difference in height of the wrinkle depth of the corrugated PMSQ particles may be.
  • the diameter of the corrugated PMSQ particles may be further increased as the addition ratio of the methyltrimethoxysilane increases.
  • the diameter of the corrugated PMSQ particles may be adjusted according to the selection of the catalyst type.
  • the catalyst comprises at least one selected from the group consisting of aminopropyltrimethoxysilane, triethylamine, ammonium hydroxide (NH 4 OH) and triethanolamine. May be
  • the catalyst includes aminopropyltrimethoxysilane, and the diameter of the corrugated PMSQ particles may be 1 ⁇ m to 6 ⁇ m.
  • the catalyst includes triethylamine, and the diameter of the corrugated PMSQ particles may be 6 ⁇ m to 8 ⁇ m.
  • the catalyst includes ammonium hydroxide (NH 4 OH), and the diameter of the corrugated PMSQ particles may be 8 ⁇ m to 30 ⁇ m.
  • the PMSQ powder according to an embodiment of the present invention includes two or more different types of silanes, the surface includes wrinkle-shaped PMSQ particles having a wrinkle shape, and the thickness of the wrinkle is 10 nm to 1000 nm, and the wrinkle The spacing is between 10 nm and 1000 nm.
  • the pleated PMSQ particles may be manufactured according to a method of manufacturing pleated PMSQ particles according to an embodiment of the present invention.
  • Functional cosmetics includes a PMSQ powder according to an embodiment of the present invention.
  • the diffuse reflection film according to an embodiment of the present invention includes a PMSQ powder according to an embodiment of the present invention.
  • 1A is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 1.
  • 1B is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 1.
  • 1C is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 2.
  • 1D is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 2.
  • 2A is a low magnification SEM image of corrugated PMSQ particles prepared according to Example 3.
  • 2B is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 3.
  • 2C is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 4.
  • 2D is a high magnification SEM image of wrinkled PMSQ particles prepared according to Example 4.
  • Example 3 is an XRD result of the wrinkled PMSQ particles of Example 1 and general PMSQ particles.
  • Example 6 is an SEM image of the wrinkled PMSQ particles of Example 1 and general PMSQ particles.
  • a method of manufacturing corrugated PMSQ particles comprises: preparing a catalyst solution by mixing a selected catalyst with an organic solvent; Preparing a reaction solution by adding two or more different silanes to the catalyst solution; And synthesizing PMSQ (polymethylsilsesquioxane) particles having wrinkles on the surface through the reaction solution.
  • PMSQ polymethylsilsesquioxane
  • the manufacturing method of the corrugated PMSQ particles according to the present invention it is possible to implement the corrugated PMSQ particles having an embossing effect by the corrugated surface and having excellent diffuse reflection properties.
  • the two or more different types of silanes methyltriethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, dimethyldiethoxysilane, normal propyl Trimethoxysilane (N-propyltrimethoxysilane), N-propyltriethoxysilane, Vinyltrimethoxysilane, Vinyltriethoxysilane, Phenyltrimethoxysilane, It may include at least two selected from the group consisting of phenyltriethoxysilane, diphenyldimethoxysilane and methylphenyldimethoxysilane.
  • the present invention is not limited thereto, and an alkylsilane-based material may be used without limitation.
  • a difference in wrinkle depth of wrinkled PMSQ particles finally produced is a result of a difference in reaction speed due to chain length and molecular weight between silanes.
  • the two or more different types of silanes are methyltriethoxysilane and methyltrimethoxysilane
  • the addition ratio of the methyltriethoxysilane and the methyltrimethoxysilane is It may be 4:1 (mole) to 1:4 (mole).
  • it may be 1: 1 (mol) to 3: 1 (mol).
  • the higher the addition ratio of the methyl trimethoxysilane, the higher the difference in height of the wrinkle depth of the corrugated PMSQ particles may be.
  • the diameter of the corrugated PMSQ particles may be further increased as the addition ratio of the methyltrimethoxysilane increases.
  • the step of preparing a catalyst solution by mixing the selected catalyst with the organic solvent may be to add distilled water, an organic solvent and a catalyst, and to mix them under a temperature condition of 40°C to 60°C.
  • the diameter of the corrugated PMSQ particles may be adjusted according to the selection of the catalyst type.
  • the diameter of the corrugated PMSQ particles finally produced is adjusted according to the selection of the catalyst type, which is a result of the difference in the reaction rate of the silane according to the catalyst type.
  • the catalyst comprises at least one selected from the group consisting of aminopropyltrimethoxysilane, triethylamine, ammonium hydroxide (NH 4 OH) and triethanolamine.
  • the present invention is not limited thereto, and may include an aminosilane-based catalyst, an amine-based catalyst, and a hydroxide-based catalyst.
  • the catalyst includes aminopropyltrimethoxysilane, and the diameter of the corrugated PMSQ particles may be 1 ⁇ m to 6 ⁇ m.
  • the catalyst includes triethylamine, and the diameter of the corrugated PMSQ particles may be 6 ⁇ m to 8 ⁇ m.
  • the catalyst includes ammonium hydroxide (NH 4 OH), and the diameter of the corrugated PMSQ particles may be 8 ⁇ m to 30 ⁇ m.
  • the size of the diameter of the corrugated PMSQ particles finally produced can be controlled by controlling the catalyst to be added. Therefore, it is possible to implement wrinkle-shaped PMSQ particles applicable to various articles such as functional cosmetics and diffuse reflection films by simply adjusting the catalyst type.
  • the step of synthesizing PMSQ (polymethylsilsesquioxane, polymethylsilsesquioxane) particles having wrinkles on the surface through the reaction solution is performed for 3 to 5 hours in a reaction solution in which two or more different silanes are added. During the reaction, it may be to synthesize PMSQ particles.
  • a filtration step; Washing step; Drying step; Grinding step; And screening step may be to further include.
  • the filtration step, the washing step, the drying step, the crushing step, and the screening step may be carried out by a conventional method, and may be changeable depending on the applied article of PMSQ particles to be manufactured.
  • the PMSQ powder according to an embodiment of the present invention includes two or more different types of silanes, the surface includes wrinkle-shaped PMSQ particles having a wrinkle shape, and the thickness of the wrinkle is 10 nm to 1000 nm, and the wrinkle The spacing is between 10 nm and 1000 nm.
  • the height difference of the wrinkle depth may be 10 nm to 2000 nm.
  • the pleated PMSQ particles may be manufactured according to a method of manufacturing pleated PMSQ particles according to an embodiment of the present invention.
  • Functional cosmetics includes a PMSQ powder according to an embodiment of the present invention.
  • PMSQ powder according to an embodiment of the present invention by including wrinkled PMSQ particles, the compatibility with silicone oil and distilled water is very good compared to the existing silicone powder, optical simulation results show a diffuse reflection effect of light compared to the existing silicone powder Is excellent In addition, the skin texture is excellent due to the embossing effect, so it is possible to implement a functional cosmetic product having an excellent wrinkle hiding effect and an uncomfortable feeling of use.
  • the diffuse reflection film according to an embodiment of the present invention includes a PMSQ powder according to an embodiment of the present invention.
  • the PMSQ powder according to an embodiment of the present invention has superior light scattering effect compared to a conventional silicone powder, and when applied to a film, it can implement a scattering film having excellent physical properties.
  • a reaction solution was prepared by adding 0.75 moles of methyltriethoxysilane (MTES) and 0.25 moles of methyltrimethoxysilane (MTMS) to the catalyst solution.
  • MTES methyltriethoxysilane
  • MTMS methyltrimethoxysilane
  • the reaction solution was reacted for 4 hours.
  • a reaction solution was prepared by adding 0.5 moles of methyltriethoxysilane (MTES) and 0.5 moles of methyltrimethoxysilane (MTMS) to the catalyst solution.
  • MTES methyltriethoxysilane
  • MTMS methyltrimethoxysilane
  • the reaction solution was reacted for 4 hours.
  • a reaction solution was prepared by adding 0.75 moles of methyltriethoxysilane (MTES) and 0.25 moles of methyltrimethoxysilane (MTMS) to the catalyst solution.
  • MTES methyltriethoxysilane
  • MTMS methyltrimethoxysilane
  • the reaction solution was reacted for 4 hours.
  • a reaction solution was prepared by adding 0.75 moles of methyltriethoxysilane (MTES) and 0.25 moles of methyltrimethoxysilane (MTMS) to the catalyst solution.
  • MTES methyltriethoxysilane
  • MTMS methyltrimethoxysilane
  • the reaction solution was reacted for 4 hours.
  • a PMSQ powder containing general PMSQ particles was prepared.
  • 1A is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 1.
  • 1B is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 1.
  • 1C is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 2.
  • 1D is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 2.
  • 2A is a low magnification SEM image of corrugated PMSQ particles prepared according to Example 3.
  • 2B is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 3.
  • 2C is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 4.
  • 2D is a high magnification SEM image of wrinkled PMSQ particles prepared according to Example 4.
  • Example 3 is an XRD result of the wrinkled PMSQ particles of Example 1 and general PMSQ particles.
  • the corrugated PMSQ particles prepared according to an embodiment of the present invention exhibit similar XRD peaks compared to the conventional PMSQ particles. That is, it is possible to implement PMSQ particles using two or more silanes.
  • the PMSQ powder of the embodiment has excellent compatibility with distilled water (D.I Water base) and silicone oil (Silicone oil base) compared to the existing PMSQ powder.
  • FIG. 6 is an SEM image of the wrinkled PMSQ particles of Example 1 and general PMSQ particles. Referring to FIG. 6, it can be seen that the corrugated PMSQ particles of Example 1 had no corrugated particles, whereas the PMSQ particles of the comparative example had no corrugated surfaces.
  • the PMSQ powder according to an embodiment of the present invention includes wrinkled PMSQ particles, so that it is very compatible with silicone oil and distilled water compared to the existing silicon powder, and the optical simulation results show that the light The diffuse reflection effect is excellent.
  • the skin texture is excellent due to the embossing effect, so it is possible to implement a functional cosmetic product having an excellent wrinkle hiding effect and an uncomfortable feeling of use.

Abstract

The present invention relates to a method for preparing wrinkle-shaped polymethylsilsesquioxane particles, and polymethylsilsesquioxane powder comprising the polymethylsilsesquioxane particles prepared thereby and, more particularly, to: a method for preparing wrinkle-shaped polymethylsilsesquioxane particles, comprising the steps of preparing a catalyst solution by mixing a selected catalyst in an organic solvent, preparing a reaction solution by adding two or more different types of silanes into the catalyst solution, and synthesizing polymethylsilsesquioxane (PMSQ) particles having wrinkles on the surface thereof by using the reaction solution; and polymethylsilsesquioxane powder comprising polymethylsilsesquioxane particles prepared thereby.

Description

주름 모양 폴리메틸실세스퀴옥세인 입자의 제조방법 및 이를 통해 제조된 폴리메틸실세스퀴옥세인 입자를 포함하는 폴리메틸실세스퀴옥세인 파우더 Method for manufacturing wrinkled polymethylsilsesquioxane particles and polymethylsilsesquioxane powder comprising polymethylsilsesquioxane particles prepared therefrom
본 발명은 주름 모양 폴리메틸실세스퀴옥세인 입자의 제조방법 및 이를 통해 제조된 폴리메틸실세스퀴옥세인 입자를 포함하는 폴리메틸실세스퀴옥세인 파우더에 관한 것이다.The present invention relates to a method for producing corrugated polymethylsilsesquioxane particles and a polymethylsilsesquioxane powder comprising polymethylsilsesquioxane particles produced therefrom.
주름을 개선하기 위한 화장품은 주름을 발생시키는 인자에 작용하여 근본적으로 주름을 없애는 기능성 화장품과 분체를 이용하여 주름 부위를 메우고 주름 부위에서 빛을 난반사 하여 일시적으로 주름 은폐효과를 갖는 화장품으로 나눌 수 있다.Cosmetics to improve wrinkles can be divided into functional cosmetics that basically remove wrinkles by acting on factors that cause wrinkles, and cosmetics that have temporary concealing effect by filling the wrinkles with light and diffused light from the wrinkles. .
주름 부위에서 난반사를 일으켜 일시적으로 주름을 가리는 화장품의 경우 과량의 분체가 첨가되어 무겁고 뻣뻣한 사용감을 가지게 되고 피부에 도포 시 백탁 현상을 유발하므로 그 사용이 제한적일 수밖에 없다. 또한, 분체가 가지고 있는 흡습, 흡유 성질 때문에 피부가 건조해지면서 피부와 밀착력이 떨어져 피부 위에서 뭉치고 들뜨는 현상이 발생하여 지속적인 효과를 나타내기 힘들다는 문제점을 가지고 있다.In the case of cosmetics that temporarily cover the wrinkles by causing diffuse reflection at the wrinkles, excessive powder is added to have a heavy and stiff feeling, and when applied to the skin, it causes cloudiness, so its use is bound to be limited. In addition, due to the moisture absorption and oil absorption properties of the powder, the skin becomes dry and the adhesive force with the skin is reduced, causing a phenomenon of clumping and excitement on the skin, and thus has a problem that it is difficult to exhibit a continuous effect.
한편, 빛의 난반사 원리는 다음과 같다. 빛이 어떤 물질에 조사되었을 때, 일부는 빛은 표면에서 반사되고 일부는 투과되게 되는데 이때 물질의 굴절률에 따라 빛은 특정 각도로 굴절되어 투과되게 된다. 아주 작은 입자의 결합으로 되어있는 물질에 빛이 조사되었을 경우 표면에 위치한 입자에서 빛의 일부는 반사되고 나머지는 특정 각도로 굴절되어 투과되게 된다. 투과된 빛은 내부의 두 번째 입자의 표면에서 같은 현상이 발생하는데, 물질의 굴절률과 내부 입자 구조에 따라 두 번째 입자 표면에서 반사된 빛은 첫 번째 입자에서 반사된 빛과 다른 각도로 반사되게 된다. 이러한 현상이 내부에 위치한 입자들 사이에서 연속적으로 일어나게 되면서 반사된 빛들이 각각의 다른 각도로 반사되어 최종적으로 빛을 난반사하게 된다.On the other hand, the principle of diffuse reflection of light is as follows. When light is irradiated to a material, part of the light is reflected from the surface, and part of it is transmitted. At this time, light is refracted at a specific angle and transmitted according to the refractive index of the material. When light is irradiated to a material composed of very small particles, a part of the light is reflected from the particles located on the surface and the rest is refracted at a specific angle and transmitted. The transmitted light has the same phenomenon on the surface of the second particle inside. Depending on the refractive index of the material and the structure of the inner particle, the light reflected from the surface of the second particle is reflected at a different angle from the light reflected from the first particle. . As this phenomenon occurs continuously between the particles located inside, the reflected lights are reflected at different angles, and finally the light is diffusely reflected.
본 발명은 상술한 문제점을 해결하기 위한 것으로, 본 발명의 목적은, 엠보싱 효과로 피부 질감이 우수하고, 우수한 난반사 특성을 가지는 주름 모양 폴리메틸실세스퀴옥세인 입자 및 이의 제조방법을 제공하는 것이다.The present invention is to solve the above-mentioned problems, the object of the present invention is to provide a wrinkle-like polymethylsilsesquioxane particles having excellent skin texture with excellent embossing effect and excellent diffuse reflection properties, and a method for manufacturing the same.
또한, 상기 주름 모양 폴리메틸실세스퀴옥세인 입자를 포함하는 폴리메틸실세스퀴옥세인 파우더를 제공하는 것이다.In addition, it is to provide a polymethylsilsesquioxane powder containing the wrinkled polymethylsilsesquioxane particles.
또한, 상기 폴리메틸실세스퀴옥세인 파우더를 포함하는 기능성 화장품을 제공하는 것이다.In addition, to provide a functional cosmetic containing the polymethylsilsesquioxane powder.
또한, 상기 폴리메틸실세스퀴옥세인 파우더를 포함하는 난반사 필름을 제공하는 것이다.In addition, to provide a diffuse reflection film comprising the polymethylsilsesquioxane powder.
그러나, 본 발명이 해결하고자 하는 과제는 이상에서 언급한 것들로 제한되지 않으며, 언급되지 않은 또 다른 과제들은 아래의 기재로부터 해당 분야 통상의 기술자에게 명확하게 이해될 수 있을 것이다.However, the problems to be solved by the present invention are not limited to those mentioned above, and other problems not mentioned will be clearly understood by those skilled in the art from the following description.
본 발명의 일 실시예에 따른 주름 모양 PMSQ 입자의 제조방법은, 유기용매에 선택된 촉매를 혼합하여 촉매 용액을 제조하는 단계; 상기 촉매 용액에 서로 다른 2 종 이상의 실란을 첨가하여 반응 용액을 제조하는 단계; 및 상기 반응 용액을 통해 표면에 주름이 형성된 PMSQ(폴리메틸실세스퀴옥세인, polymethylsilsesquioxane) 입자를 합성하는 단계;를 포함한다.A method of manufacturing corrugated PMSQ particles according to an embodiment of the present invention comprises: preparing a catalyst solution by mixing a selected catalyst with an organic solvent; Preparing a reaction solution by adding two or more different silanes to the catalyst solution; And synthesizing PMSQ (polymethylsilsesquioxane) particles having wrinkles on the surface through the reaction solution.
일 측면에 따르면, 상기 서로 다른 2 종 이상의 실란은, 메틸트리에톡시실란 (methyltriethoxysilane), 메틸트리메톡시실란 (methyltrimethoxysilane), 디메틸디메톡시실란 (dimethyldimethoxysilane), 디메틸디에톡시실란 (dimethyldiethoxysilane), 노르말프로필트리메톡시실란 (N-propyltrimethoxysilane), 노르말프로필트리에톡시실란 (N-propyltriethoxysilane), 비닐트리메톡시실란 (Vinyltrimethoxysilane), 비닐트리에톡시시란 (Vinyltriethoxysilane), 페닐트리메톡시실란 (Phenyltrimethoxysilane), 페닐트리에톡시실란 (Phenyltriethoxysilane), 디페닐디메톡시실란 (Diphenyldimethoxysilane) 및 메틸페닐디메톡시실란 (Methylphenyldimethoxysilane)으로 이루어진 군으로부터 선택된 적어도 2 종을 포함하는 것일 수 있다.According to one aspect, the two or more different types of silanes, methyltriethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, dimethyldiethoxysilane, normal propyl Trimethoxysilane (N-propyltrimethoxysilane), N-propyltriethoxysilane, Vinyltrimethoxysilane, Vinyltriethoxysilane, Phenyltrimethoxysilane, It may include at least two selected from the group consisting of phenyltriethoxysilane, diphenyldimethoxysilane and methylphenyldimethoxysilane.
일 측면에 따르면, 상기 서로 다른 2종 이상의 실란은, 메틸트리에톡시실란 (methyltriethoxysilane) 및 메틸트리메톡시실란(methyltrimethoxysilane)이고, 상기 메틸트리에톡시실란 및 상기 메틸트리메톡시실란의 첨가 비율은 4 : 1 (몰) 내지 1 : 4 (몰)인 것일 수 있다.According to one aspect, the two or more different types of silanes are methyltriethoxysilane and methyltrimethoxysilane, and the addition ratio of the methyltriethoxysilane and the methyltrimethoxysilane is It may be 4:1 (mole) to 1:4 (mole).
일 측면에 따르면, 상기 메틸트리메톡시실란의 첨가 비율이 올라갈수록 상기 주름 모양 PMSQ 입자의 주름 깊이의 높낮이차가 더욱 증가하는 것일 수 있다.According to one aspect, the higher the addition ratio of the methyl trimethoxysilane, the higher the difference in height of the wrinkle depth of the corrugated PMSQ particles may be.
일 측면에 따르면, 상기 메틸트리메톡시실란의 첨가 비율이 올라갈수록 상기 주름 모양 PMSQ 입자의 직경이 더욱 증가하는 것일 수 있다.According to one aspect, the diameter of the corrugated PMSQ particles may be further increased as the addition ratio of the methyltrimethoxysilane increases.
일 측면에 따르면, 상기 촉매 종류의 선택에 따라 상기 주름 모양 PMSQ 입자의 직경이 조절되는 것일 수 있다.According to one aspect, the diameter of the corrugated PMSQ particles may be adjusted according to the selection of the catalyst type.
일 측면에 따르면, 상기 촉매는, 아미노프로필트리메톡시실란 (Aminopropyltrimethoxysilane), 트리에틸아민(Triethylamine), 수산화 암모늄(NH 4OH) 및 트리에탄올아민(Triethanolamine)으로 이루어진 군으로부터 선택되는 적어도 하나를 포함하는 것일 수 있다.According to one aspect, the catalyst comprises at least one selected from the group consisting of aminopropyltrimethoxysilane, triethylamine, ammonium hydroxide (NH 4 OH) and triethanolamine. May be
일 측면에 따르면, 상기 촉매는 아미노프로필트리메톡시실란 (Aminopropyltrimethoxysilane)을 포함하고, 상기 주름 모양 PMSQ 입자의 직경은 1 ㎛ 내지 6 ㎛인 것일 수 있다.According to one aspect, the catalyst includes aminopropyltrimethoxysilane, and the diameter of the corrugated PMSQ particles may be 1 μm to 6 μm.
일 측면에 따르면, 상기 촉매는 트리에틸아민(Triethylamine)을 포함하고, 상기 주름 모양 PMSQ 입자의 직경은 6 ㎛ 내지 8 ㎛인 것일 수 있다.According to one aspect, the catalyst includes triethylamine, and the diameter of the corrugated PMSQ particles may be 6 μm to 8 μm.
일 측면에 따르면, 상기 촉매는 수산화 암모늄(NH 4OH)을 포함하고, 상기 주름 모양 PMSQ 입자의 직경은 8 ㎛ 내지 30 ㎛인 것일 수 있다.According to one aspect, the catalyst includes ammonium hydroxide (NH 4 OH), and the diameter of the corrugated PMSQ particles may be 8 μm to 30 μm.
본 발명의 일 실시예에 따른 PMSQ 파우더는, 서로 다른 2 종 이상의 실란을 포함하고, 표면이 주름 형태인 주름 모양 PMSQ 입자를 포함하고, 상기 주름의 두께가 10 nm 내지 1000 nm이고, 상기 주름의 간격이 10 nm 내지 1000 nm인 것이다.The PMSQ powder according to an embodiment of the present invention includes two or more different types of silanes, the surface includes wrinkle-shaped PMSQ particles having a wrinkle shape, and the thickness of the wrinkle is 10 nm to 1000 nm, and the wrinkle The spacing is between 10 nm and 1000 nm.
일 측면에 따르면, 상기 주름 모양 PMSQ 입자는, 본 발명의 일 실시예에 따른 주름 모양 PMSQ 입자의 제조방법에 따라 제조된 것일 수 있다.According to an aspect, the pleated PMSQ particles may be manufactured according to a method of manufacturing pleated PMSQ particles according to an embodiment of the present invention.
본 발명의 일 실시예에 따른 기능성 화장품은, 본 발명의 일 실시예에 따른 PMSQ 파우더를 포함한다.Functional cosmetics according to an embodiment of the present invention, includes a PMSQ powder according to an embodiment of the present invention.
본 발명의 일 실시예에 따른 난반사 필름은, 본 발명의 일 실시예에 따른 PMSQ 파우더를 포함한다.The diffuse reflection film according to an embodiment of the present invention includes a PMSQ powder according to an embodiment of the present invention.
본 발명에 따른 주름 모양 폴리메틸실세스퀴옥세인 입자의 제조방법에 따르면, 주름진 표면에 의해 엠보싱 효과를 가지고, 우수한 난반사 특성을 가지는 주름 모양 폴리메틸실세스퀴옥세인 입자를 구현할 수 있다.According to the method for producing wrinkled polymethylsilsesquioxane particles according to the present invention, it is possible to implement wrinkled polymethylsilsesquioxane particles having an embossing effect by a wrinkled surface and having excellent diffuse reflection properties.
또한, 엠보싱 효과로 피부 질감이 우수하고, 우수한 난반사 특성으로 주름 은폐 효과가 뛰어난 기능성 화장품을 구현할 수 있다.In addition, it is possible to implement a functional cosmetic product having excellent skin texture due to the embossing effect and excellent anti-wrinkle effect with excellent diffuse reflection properties.
도 1a는 실시예 1에 따라 제조된 주름 모양 PMSQ 입자의 저배율 SEM 이미지이다.1A is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 1.
도 1b는 실시예 1에 따라 제조된 주름 모양 PMSQ 입자의 고배율 SEM 이미지이다.1B is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 1.
도 1c는 실시예 2에 따라 제조된 주름 모양 PMSQ 입자의 저배율 SEM 이미지이다.1C is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 2.
도 1d는 실시예 2에 따라 제조된 주름 모양 PMSQ 입자의 고배율 SEM 이미지이다.1D is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 2.
도 2a는 실시예 3에 따라 제조된 주름 모양 PMSQ 입자의 저배율 SEM 이미지이다.2A is a low magnification SEM image of corrugated PMSQ particles prepared according to Example 3.
도 2b는 실시예 3에 따라 제조된 주름 모양 PMSQ 입자의 고배율 SEM 이미지이다.2B is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 3.
도 2c는 실시예 4에 따라 제조된 주름 모양 PMSQ 입자의 저배율 SEM 이미지이다.2C is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 4.
도 2d는 실시예 4에 따라 제조된 주름 모양 PMSQ 입자의 고배율 SEM 이미지이다.2D is a high magnification SEM image of wrinkled PMSQ particles prepared according to Example 4.
도 3은 실시예 1의 주름 모양 PMSQ 입자 및 일반적인 PMSQ 입자의 XRD 결과이다.3 is an XRD result of the wrinkled PMSQ particles of Example 1 and general PMSQ particles.
도 4는 실시예 1의 주름 모양 PMSQ 입자의 FIB(Focused Ion Beam) 측정 결과이다.4 is a result of measuring the FIB (Focused Ion Beam) of the wrinkled PMSQ particles of Example 1.
도 5는 실시예 1의 주름 모양 PMSQ 입자를 포함하는 실시예의 PMSQ 파우더 및 일반적인 PMSQ 입자를 포함하는 비교예의 PMSQ 파우더의 혼용성을 비교한 이미지이다.5 is an image comparing the compatibility of the PMSQ powder of the comparative example containing the PMSQ powder and the general PMSQ particles of the embodiment containing the wrinkled PMSQ particles of Example 1.
도 6은 실시예 1의 주름 모양 PMSQ 입자 및 일반적인 PMSQ 입자의 SEM 이미지이다.6 is an SEM image of the wrinkled PMSQ particles of Example 1 and general PMSQ particles.
이하 첨부된 도면을 참조하여 본 발명의 실시예들을 상세히 설명한다. 본 발명을 설명함에 있어서, 관련된 공지 기능 또는 구성에 대한 구체적인 설명이 본 발명의 요지를 불필요하게 흐릴 수 있다고 판단되는 경우에는 그 상세한 설명을 생략할 것이다. 또한, 본 명세서에서 사용되는 용어들은 본 발명의 바람직한 실시예를 적절히 표현하기 위해 사용된 용어들로서, 이는 사용자, 운용자의 의도 또는 본 발명이 속하는 분야의 관례 등에 따라 달라질 수 있다. 따라서, 본 용어들에 대한 정의는 본 명세서 전반에 걸친 내용을 토대로 내려져야 할 것이다. 각 도면에 제시된 동일한 참조 부호는 동일한 부재를 나타낸다.Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. In describing the present invention, when it is determined that a detailed description of related known functions or configurations may unnecessarily obscure the subject matter of the present invention, the detailed description will be omitted. In addition, terms used in the present specification are terms used to appropriately represent a preferred embodiment of the present invention, which may vary depending on a user, an operator's intention, or a custom in the field to which the present invention pertains. Therefore, definitions of these terms should be made based on the contents throughout the specification. The same reference numerals in each drawing denote the same members.
명세서 전체에서, 어떤 부재가 다른 부재 "상에" 위치하고 있다고 할 때, 이는 어떤 부재가 다른 부재에 접해 있는 경우뿐 아니라 두 부재 사이에 또 다른 부재가 존재하는 경우도 포함한다.Throughout the specification, when one member is positioned “on” another member, this includes not only the case where one member abuts another member, but also the case where another member exists between the two members.
명세서 전체에서, 어떤 부분이 어떤 구성요소를 "포함"한다고 할 때, 이는 다른 구성요소를 제외하는 것이 아니라 다른 구성 요소를 더 포함할 수 있는 것을 의미한다.Throughout the specification, when a part “includes” a certain component, it means that the other component may be further included instead of excluding the other component.
이하, 본 발명의 주름 모양 폴리메틸실세스퀴옥세인 입자의 제조방법 및 이를 통해 제조된 폴리메틸실세스퀴옥세인 입자를 포함하는 폴리메틸실세스퀴옥세인 파우더에 대하여 실시예 및 도면을 참조하여 구체적으로 설명하도록 한다. 그러나, 본 발명이 이러한 실시예 및 도면에 제한되는 것은 아니다.Hereinafter, with reference to the examples and drawings for the method of manufacturing the wrinkle-like polymethylsilsesquioxane particles of the present invention and the polymethylsilsesquioxane powder comprising the polymethylsilsesquioxane particles produced therefrom in detail Explain. However, the present invention is not limited to these examples and drawings.
본 발명의 일 실시예에 따른 주름 모양 PMSQ 입자의 제조방법은, 유기용매에 선택된 촉매를 혼합하여 촉매 용액을 제조하는 단계; 상기 촉매 용액에 서로 다른 2 종 이상의 실란을 첨가하여 반응 용액을 제조하는 단계; 및 상기 반응 용액을 통해 표면에 주름이 형성된 PMSQ(폴리메틸실세스퀴옥세인, polymethylsilsesquioxane) 입자를 합성하는 단계;를 포함한다.A method of manufacturing corrugated PMSQ particles according to an embodiment of the present invention comprises: preparing a catalyst solution by mixing a selected catalyst with an organic solvent; Preparing a reaction solution by adding two or more different silanes to the catalyst solution; And synthesizing PMSQ (polymethylsilsesquioxane) particles having wrinkles on the surface through the reaction solution.
본 발명에 따른 주름 모양 PMSQ 입자의 제조방법에 따르면, 주름진 표면에 의해 엠보싱 효과를 가지고, 우수한 난반사 특성을 가지는 주름 모양 PMSQ 입자를 구현할 수 있다.According to the manufacturing method of the corrugated PMSQ particles according to the present invention, it is possible to implement the corrugated PMSQ particles having an embossing effect by the corrugated surface and having excellent diffuse reflection properties.
일 측면에 따르면, 상기 서로 다른 2 종 이상의 실란은, 메틸트리에톡시실란 (methyltriethoxysilane), 메틸트리메톡시실란 (methyltrimethoxysilane), 디메틸디메톡시실란 (dimethyldimethoxysilane), 디메틸디에톡시실란 (dimethyldiethoxysilane), 노르말프로필트리메톡시실란 (N-propyltrimethoxysilane), 노르말프로필트리에톡시실란 (N-propyltriethoxysilane), 비닐트리메톡시실란 (Vinyltrimethoxysilane), 비닐트리에톡시시란 (Vinyltriethoxysilane), 페닐트리메톡시실란 (Phenyltrimethoxysilane), 페닐트리에톡시실란 (Phenyltriethoxysilane), 디페닐디메톡시실란 (Diphenyldimethoxysilane) 및 메틸페닐디메톡시실란 (Methylphenyldimethoxysilane)으로 이루어진 군으로부터 선택된 적어도 2 종을 포함하는 것일 수 있다. 다만, 이에 한정되지 않으며 알킬실란 계열의 물질이라면 제한없이 사용할 수 있다.According to one aspect, the two or more different types of silanes, methyltriethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, dimethyldiethoxysilane, normal propyl Trimethoxysilane (N-propyltrimethoxysilane), N-propyltriethoxysilane, Vinyltrimethoxysilane, Vinyltriethoxysilane, Phenyltrimethoxysilane, It may include at least two selected from the group consisting of phenyltriethoxysilane, diphenyldimethoxysilane and methylphenyldimethoxysilane. However, the present invention is not limited thereto, and an alkylsilane-based material may be used without limitation.
서로 다른 2 종 이상의 실란 원료의 몰비에 따라 최종적으로 제조되는 주름 모양 PMSQ 입자의 주름 골 깊이 차이가 발생하며, 이는 실란 간의 사슬 길이 및 분자량에 의한 반응 속도의 차이에 인한 결과이다.According to the molar ratio of two or more different types of silane raw materials, a difference in wrinkle depth of wrinkled PMSQ particles finally produced is a result of a difference in reaction speed due to chain length and molecular weight between silanes.
일 측면에 따르면, 상기 서로 다른 2종 이상의 실란은, 메틸트리에톡시실란 (methyltriethoxysilane) 및 메틸트리메톡시실란(methyltrimethoxysilane)이고, 상기 메틸트리에톡시실란 및 상기 메틸트리메톡시실란의 첨가 비율은 4 : 1 (몰) 내지 1 : 4 (몰)인 것일 수 있다. 바람직하게는 1 : 1 (몰) 내지 3 : 1 (몰)인 것일 수 있다. 메틸트리에톡시실란 (methyltriethoxysilane) 및 메틸트리메톡시실란(methyltrimethoxysilane)의 첨가 비율이 상기 조건을 만족할 경우, 엠보싱 효과를 가지고, 우수한 난반사 특성을 가지는 주름 모양 PMSQ 입자를 구현할 수 있다.According to one aspect, the two or more different types of silanes are methyltriethoxysilane and methyltrimethoxysilane, and the addition ratio of the methyltriethoxysilane and the methyltrimethoxysilane is It may be 4:1 (mole) to 1:4 (mole). Preferably it may be 1: 1 (mol) to 3: 1 (mol). When the addition ratio of methyltriethoxysilane and methyltrimethoxysilane satisfies the above conditions, it has embossing effect and can realize wrinkle-shaped PMSQ particles having excellent diffuse reflection properties.
일 측면에 따르면, 상기 메틸트리메톡시실란의 첨가 비율이 올라갈수록 상기 주름 모양 PMSQ 입자의 주름 깊이의 높낮이차가 더욱 증가하는 것일 수 있다.According to one aspect, the higher the addition ratio of the methyl trimethoxysilane, the higher the difference in height of the wrinkle depth of the corrugated PMSQ particles may be.
일 측면에 따르면, 상기 메틸트리메톡시실란의 첨가 비율이 올라갈수록 상기 주름 모양 PMSQ 입자의 직경이 더욱 증가하는 것일 수 있다.According to one aspect, the diameter of the corrugated PMSQ particles may be further increased as the addition ratio of the methyltrimethoxysilane increases.
일반적으로 실란을 출발물질로 사용하여 PMSQ 입자 합성 시 반응 속도가 빠를수록 입자 크기는 커지는 경향이 있다. 메틸트리메톡시실란의 첨가 비율이 올라갈수록 PMSQ 입자 직경이 커지는 이유는 메틸트리메톡시실란이 메틸트리에톡시실란보다 반응 속도가 빠르기 때문이다.In general, the faster the reaction rate when synthesizing PMSQ particles using silane as a starting material, the larger the particle size tends to be. The reason why the PMSQ particle diameter increases as the addition ratio of methyltrimethoxysilane increases is that methyltrimethoxysilane has a faster reaction rate than methyltriethoxysilane.
즉, 실란 원료의 첨가 비율을 조절하여 최종적으로 제조되는 주름 모양 PMSQ 입자의 주름 골 깊이를 조절할 수 있으며, 주름 모양 PMSQ 입자의 직경의 크기를 조절할 수 있다. 따라서, 실란 원료의 첨가 비율을 조절하는 것만으로 기능성 화장품, 난반사 필름 등의 다양한 물품에 적용 가능한 주름 모양 PMSQ 입자를 구현할 수 있다.That is, it is possible to control the addition ratio of the silane raw material to control the depth of the wrinkles of the corrugated PMSQ particles that are finally manufactured, and to control the size of the diameter of the corrugated PMSQ particles. Therefore, it is possible to realize wrinkle-shaped PMSQ particles applicable to various articles such as functional cosmetics and diffuse reflection films by simply adjusting the addition ratio of the silane raw material.
일 측면에 따르면, 상기 유기용매에 선택된 촉매를 혼합하여 촉매 용액을 제조하는 단계는, 증류수, 유기용매 및 촉매를 넣고 40 ℃ 내지 60 ℃의 온도 조건으로 혼합하는 것일 수 있다. According to one aspect, the step of preparing a catalyst solution by mixing the selected catalyst with the organic solvent may be to add distilled water, an organic solvent and a catalyst, and to mix them under a temperature condition of 40°C to 60°C.
일 측면에 따르면, 상기 유기용매에 선택된 촉매를 혼합하여 촉매 용액을 제조하는 단계는, 증류수 : 에탄올 : 촉매 = 4 : 2 : 0.1 (몰)의 비율로 혼합하는 것일 수 있다.According to an aspect, the step of preparing a catalyst solution by mixing the catalyst selected with the organic solvent may be mixing at a ratio of distilled water:ethanol:catalyst=4:2:0.1 (mol).
일 측면에 따르면, 상기 촉매 종류의 선택에 따라 상기 주름 모양 PMSQ 입자의 직경이 조절되는 것일 수 있다.According to one aspect, the diameter of the corrugated PMSQ particles may be adjusted according to the selection of the catalyst type.
촉매 종류의 선택에 따라 최종적으로 제조되는 주름 모양 PMSQ 입자의 직경이 조절되며, 이는 촉매 종류에 따른 실란의 반응 속도 차이에 인한 결과이다.The diameter of the corrugated PMSQ particles finally produced is adjusted according to the selection of the catalyst type, which is a result of the difference in the reaction rate of the silane according to the catalyst type.
일 측면에 따르면, 상기 촉매는, 아미노프로필트리메톡시실란 (Aminopropyltrimethoxysilane), 트리에틸아민(Triethylamine), 수산화 암모늄(NH 4OH) 및 트리에탄올아민(Triethanolamine)으로 이루어진 군으로부터 선택되는 적어도 하나를 포함하는 것일 수 있다. 다만, 이에 한정되지 않으며 아미노실란 계열 촉매, 아민 계열 촉매, 수산화염 계열 촉매 등을 포함하는 것일 수 있다.According to one aspect, the catalyst comprises at least one selected from the group consisting of aminopropyltrimethoxysilane, triethylamine, ammonium hydroxide (NH 4 OH) and triethanolamine. May be However, the present invention is not limited thereto, and may include an aminosilane-based catalyst, an amine-based catalyst, and a hydroxide-based catalyst.
일 측면에 따르면, 상기 촉매는 아미노프로필트리메톡시실란 (Aminopropyltrimethoxysilane)을 포함하고, 상기 주름 모양 PMSQ 입자의 직경은 1 ㎛ 내지 6 ㎛인 것일 수 있다.According to one aspect, the catalyst includes aminopropyltrimethoxysilane, and the diameter of the corrugated PMSQ particles may be 1 μm to 6 μm.
일 측면에 따르면, 상기 촉매는 트리에틸아민(Triethylamine)을 포함하고, 상기 주름 모양 PMSQ 입자의 직경은 6 ㎛ 내지 8 ㎛인 것일 수 있다.According to one aspect, the catalyst includes triethylamine, and the diameter of the corrugated PMSQ particles may be 6 μm to 8 μm.
일 측면에 따르면, 상기 촉매는 수산화 암모늄(NH 4OH)을 포함하고, 상기 주름 모양 PMSQ 입자의 직경은 8 ㎛ 내지 30 ㎛인 것일 수 있다.According to one aspect, the catalyst includes ammonium hydroxide (NH 4 OH), and the diameter of the corrugated PMSQ particles may be 8 μm to 30 μm.
즉, 첨가되는 촉매를 조절하여 최종적으로 제조되는 주름 모양 PMSQ 입자의 직경의 크기를 조절할 수 있다. 따라서, 촉매 종류를 조절하는 것만으로 기능성 화장품, 난반사 필름 등의 다양한 물품에 적용 가능한 주름 모양 PMSQ 입자를 구현할 수 있다.That is, the size of the diameter of the corrugated PMSQ particles finally produced can be controlled by controlling the catalyst to be added. Therefore, it is possible to implement wrinkle-shaped PMSQ particles applicable to various articles such as functional cosmetics and diffuse reflection films by simply adjusting the catalyst type.
일 측면에 따르면, 상기 반응 용액을 통해 표면에 주름이 형성된 PMSQ(폴리메틸실세스퀴옥세인, polymethylsilsesquioxane) 입자를 합성하는 단계는, 서로 다른 2 종 이상의 실란이 첨가된 반응 용액을 3 시간 내지 5 시간동안 반응시켜, PMSQ 입자를 합성하는 것일 수 있다.According to one aspect, the step of synthesizing PMSQ (polymethylsilsesquioxane, polymethylsilsesquioxane) particles having wrinkles on the surface through the reaction solution is performed for 3 to 5 hours in a reaction solution in which two or more different silanes are added. During the reaction, it may be to synthesize PMSQ particles.
일 측면에 따르면, 상기 반응 용액을 통해 표면에 주름이 형성된 PMSQ(폴리메틸실세스퀴옥세인, polymethylsilsesquioxane) 입자를 합성하는 단계 이후, 여과 단계; 세척 단계; 건조 단계; 분쇄 단계; 및 선별 단계;를 더 포함하는 것일 수 있다.According to one aspect, after the step of synthesizing PMSQ (polymethylsilsesquioxane, polymethylsilsesquioxane) particles with wrinkles on the surface through the reaction solution, a filtration step; Washing step; Drying step; Grinding step; And screening step; may be to further include.
상기 여과 단계, 세척 단계, 건조 단계, 분쇄 단계 및 선별 단계는 통상적인 방법으로 실시되는 것일 수 있으며, 제조되는 PMSQ 입자의 적용 물품에 따라 변경 가능한 것일 수 있다.The filtration step, the washing step, the drying step, the crushing step, and the screening step may be carried out by a conventional method, and may be changeable depending on the applied article of PMSQ particles to be manufactured.
본 발명의 일 실시예에 따른 PMSQ 파우더는, 서로 다른 2 종 이상의 실란을 포함하고, 표면이 주름 형태인 주름 모양 PMSQ 입자를 포함하고, 상기 주름의 두께가 10 nm 내지 1000 nm이고, 상기 주름의 간격이 10 nm 내지 1000 nm인 것이다.The PMSQ powder according to an embodiment of the present invention includes two or more different types of silanes, the surface includes wrinkle-shaped PMSQ particles having a wrinkle shape, and the thickness of the wrinkle is 10 nm to 1000 nm, and the wrinkle The spacing is between 10 nm and 1000 nm.
일 측면에 따르면, 상기 주름 깊이의 높낮이차는 10 nm 내지 2000 nm인 것일 수 있다.According to one aspect, the height difference of the wrinkle depth may be 10 nm to 2000 nm.
일 측면에 따르면, 상기 주름 모양 PMSQ 입자는, 본 발명의 일 실시예에 따른 주름 모양 PMSQ 입자의 제조방법에 따라 제조된 것일 수 있다.According to an aspect, the pleated PMSQ particles may be manufactured according to a method of manufacturing pleated PMSQ particles according to an embodiment of the present invention.
상술한 바와 같이, 제조과정에서 실란 원료의 첨가 비율 및 촉매의 종류를 조절하여, 상기 주름의 두께, 간격 및 주름 깊이의 높낮이차를 조절할 수 있으며, 실란 원료의 첨가 비율 및 촉매의 종류를 조절하는 것만으로 기능성 화장품, 난반사 필름 등의 다양한 물품에 적용 가능한 주름 모양 PMSQ 입자를 구현할 수 있다.As described above, by adjusting the addition ratio of the silane raw material and the type of catalyst in the manufacturing process, it is possible to control the height difference between the thickness of the wrinkles, the spacing and the wrinkle depth, and to control the addition ratio of the silane raw material and the type of catalyst. Wrinkle-shaped PMSQ particles that can be applied to various articles such as functional cosmetics and diffuse reflection films can be realized by simply using them.
본 발명의 일 실시예에 따른 기능성 화장품은, 본 발명의 일 실시예에 따른 PMSQ 파우더를 포함한다.Functional cosmetics according to an embodiment of the present invention, includes a PMSQ powder according to an embodiment of the present invention.
본 발명의 일 실시예에 따른 PMSQ 파우더는 주름 모양 PMSQ 입자를 포함함으로써, 기존 실리콘 파우더와 비교하여 실리콘 오일 및 증류수와의 혼용성이 매우 우수하며, 광학 시뮬레이션 결과 기존 실리콘 파우더에 비해 빛의 난반사 효과가 뛰어나다. 또한, 엠보싱 효과로 피부 질감이 우수하여, 주름 은폐 효과가 뛰어나면서도 사용감이 불편하지 않은 기능성 화장품을 구현할 수 있다.PMSQ powder according to an embodiment of the present invention, by including wrinkled PMSQ particles, the compatibility with silicone oil and distilled water is very good compared to the existing silicone powder, optical simulation results show a diffuse reflection effect of light compared to the existing silicone powder Is excellent In addition, the skin texture is excellent due to the embossing effect, so it is possible to implement a functional cosmetic product having an excellent wrinkle hiding effect and an uncomfortable feeling of use.
본 발명의 일 실시예에 따른 난반사 필름은, 본 발명의 일 실시예에 따른 PMSQ 파우더를 포함한다.The diffuse reflection film according to an embodiment of the present invention includes a PMSQ powder according to an embodiment of the present invention.
본 발명의 일 실시예에 따른 PMSQ 파우더는 기존 실리콘 파우더에 비해 빛의 난반사 효과가 뛰어나며, 이를 필름에 적용하였을 경우, 물성이 뛰어난 난반사 필름을 구현할 수 있다.The PMSQ powder according to an embodiment of the present invention has superior light scattering effect compared to a conventional silicone powder, and when applied to a film, it can implement a scattering film having excellent physical properties.
이하, 실시예 및 비교예에 의하여 본 발명을 더욱 상세히 설명하고자 한다.Hereinafter, the present invention will be described in more detail by examples and comparative examples.
단, 하기 실시예는 본 발명을 예시하기 위한 것일 뿐, 본 발명의 내용이 하기 실시예에 한정되는 것은 아니다.However, the following examples are only for illustrating the present invention, and the contents of the present invention are not limited to the following examples.
실시예 1Example 1
2L 4구 반응기에 증류수 40 몰과 에탄올 20 몰을 넣고 혼합 후 아미노프로필트리메톡시실란(Aminopropyltrimethoxysilane) 0.1 몰을 넣고 50 ℃에서 200 rpm으로 혼합하여 촉매 용액을 제조하였다.In a 2L 4-neck reactor, 40 moles of distilled water and 20 moles of ethanol were added, and after mixing, 0.1 moles of aminopropyltrimethoxysilane was added and mixed at 50°C at 200 rpm to prepare a catalyst solution.
상기 촉매 용액에 MTES(methyltriethoxysilane) 0.75 몰과 MTMS(methyltrimethoxysilane) 0.25 몰을 첨가하여 반응 용액을 제조하였다.A reaction solution was prepared by adding 0.75 moles of methyltriethoxysilane (MTES) and 0.25 moles of methyltrimethoxysilane (MTMS) to the catalyst solution.
상기 반응 용액을 4 시간동안 반응시켰다.The reaction solution was reacted for 4 hours.
반응 종료 후 여과, 세척, 건조, 분쇄, 선별 공정을 거쳐 주름 모양 PMSQ 입자를 제조하였다.After the reaction was completed, filtration, washing, drying, pulverization, and screening processes were performed to prepare corrugated PMSQ particles.
실시예 2Example 2
2L 4구 반응기에 증류수 40 몰과 에탄올 20 몰을 넣고 혼합 후 아미노프로필트리메톡시실란(Aminopropyltrimethoxysilane) 0.1 몰을 넣고 50 ℃에서 200 rpm으로 혼합하여 촉매 용액을 제조하였다.In a 2L 4-neck reactor, 40 moles of distilled water and 20 moles of ethanol were added, and after mixing, 0.1 moles of aminopropyltrimethoxysilane was added and mixed at 50°C at 200 rpm to prepare a catalyst solution.
상기 촉매 용액에 MTES(methyltriethoxysilane) 0.5 몰과 MTMS(methyltrimethoxysilane) 0.5 몰을 첨가하여 반응 용액을 제조하였다.A reaction solution was prepared by adding 0.5 moles of methyltriethoxysilane (MTES) and 0.5 moles of methyltrimethoxysilane (MTMS) to the catalyst solution.
상기 반응 용액을 4 시간동안 반응시켰다.The reaction solution was reacted for 4 hours.
반응 종료 후 여과, 세척, 건조, 분쇄, 선별 공정을 거쳐 주름 모양 PMSQ 입자를 제조하였다.After the reaction was completed, filtration, washing, drying, pulverization, and screening processes were performed to prepare corrugated PMSQ particles.
실시예 3Example 3
2L 4구 반응기에 증류수 40 몰과 에탄올 20 몰을 넣고 혼합 후 트리에틸아민(Triethylamine) 0.1 몰을 넣고 50 ℃에서 200 rpm으로 혼합하여 촉매 용액을 제조하였다.In a 2L 4-neck reactor, 40 moles of distilled water and 20 moles of ethanol were added, and after mixing, 0.1 moles of triethylamine was added and mixed at 200°C at 200 rpm to prepare a catalyst solution.
상기 촉매 용액에 MTES(methyltriethoxysilane) 0.75 몰과 MTMS(methyltrimethoxysilane) 0.25 몰을 첨가하여 반응 용액을 제조하였다.A reaction solution was prepared by adding 0.75 moles of methyltriethoxysilane (MTES) and 0.25 moles of methyltrimethoxysilane (MTMS) to the catalyst solution.
상기 반응 용액을 4 시간동안 반응시켰다.The reaction solution was reacted for 4 hours.
반응 종료 후 여과, 세척, 건조, 분쇄, 선별 공정을 거쳐 주름 모양 PMSQ 입자를 제조하였다.After the reaction was completed, filtration, washing, drying, pulverization, and screening processes were performed to prepare corrugated PMSQ particles.
실시예 4Example 4
2L 4구 반응기에 증류수 40 몰과 에탄올 20 몰을 넣고 혼합 후 수산화 암모늄(NH 4OH) 0.1 몰을 넣고 50 ℃에서 200 rpm으로 혼합하여 촉매 용액을 제조하였다.In a 2L 4-neck reactor, 40 moles of distilled water and 20 moles of ethanol were added, and after mixing, 0.1 mole of ammonium hydroxide (NH 4 OH) was added and mixed at 200°C at 200 rpm to prepare a catalyst solution.
상기 촉매 용액에 MTES(methyltriethoxysilane) 0.75 몰과 MTMS(methyltrimethoxysilane) 0.25 몰을 첨가하여 반응 용액을 제조하였다.A reaction solution was prepared by adding 0.75 moles of methyltriethoxysilane (MTES) and 0.25 moles of methyltrimethoxysilane (MTMS) to the catalyst solution.
상기 반응 용액을 4 시간동안 반응시켰다.The reaction solution was reacted for 4 hours.
반응 종료 후 여과, 세척, 건조, 분쇄, 선별 공정을 거쳐 주름 모양 PMSQ 입자를 제조하였다.After the reaction was completed, filtration, washing, drying, pulverization, and screening processes were performed to prepare corrugated PMSQ particles.
비교예Comparative example
일반적인 PMSQ 입자를 포함하는 PMSQ 파우더를 준비하였다.A PMSQ powder containing general PMSQ particles was prepared.
도 1a는 실시예 1에 따라 제조된 주름 모양 PMSQ 입자의 저배율 SEM 이미지이다. 1A is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 1.
도 1b는 실시예 1에 따라 제조된 주름 모양 PMSQ 입자의 고배율 SEM 이미지이다. 1B is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 1.
도 1c는 실시예 2에 따라 제조된 주름 모양 PMSQ 입자의 저배율 SEM 이미지이다. 1C is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 2.
도 1d는 실시예 2에 따라 제조된 주름 모양 PMSQ 입자의 고배율 SEM 이미지이다. 1D is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 2.
도 2a는 실시예 3에 따라 제조된 주름 모양 PMSQ 입자의 저배율 SEM 이미지이다.2A is a low magnification SEM image of corrugated PMSQ particles prepared according to Example 3.
도 2b는 실시예 3에 따라 제조된 주름 모양 PMSQ 입자의 고배율 SEM 이미지이다.2B is a high magnification SEM image of corrugated PMSQ particles prepared according to Example 3.
도 2c는 실시예 4에 따라 제조된 주름 모양 PMSQ 입자의 저배율 SEM 이미지이다.2C is a low magnification SEM image of wrinkled PMSQ particles prepared according to Example 4.
도 2d는 실시예 4에 따라 제조된 주름 모양 PMSQ 입자의 고배율 SEM 이미지이다.2D is a high magnification SEM image of wrinkled PMSQ particles prepared according to Example 4.
도 1a 내지 도1d, 도 2a 내지 도 2d를 참조하면, 모든 PMSQ 입자 표면에 주름 모양이 형성되는 것을 알 수 있다. 즉, 엠보싱 효과로 피부 질감이 우수한 주름 모양 PMSQ 입자가 구현된 것이다.1A to 1D and 2A to 2D, it can be seen that wrinkles are formed on the surfaces of all PMSQ particles. That is, the wrinkle-like PMSQ particles having excellent skin texture are embodied by the embossing effect.
또한, MTES 함량 대비 MTMS 함량이 증가할수록 주름 모양 PMSQ 입자의 주름 깊이의 높낮이차가 더욱 증가하는 것을 알 수 있으며, MTES 함량 대비 MTMS 함량이 증가할수록 주름 모양 PMSQ 입자의 직경이 증가하는 것을 알 수 있다. (실시예 1의 PMSQ 입자 직경: 2.6 ㎛ 내지 2.7 ㎛, 실시예 2의 PMSQ 입자 직경: 3.3 ㎛ 내지 5.2 ㎛)In addition, it can be seen that as the MTMS content compared to the MTES content increases, the difference in height of the wrinkle depth of the corrugated PMSQ particles increases, and as the MTMS content relative to the MTES content increases, the diameter of the corrugated PMSQ particles increases. (PMSQ particle diameter of Example 1: 2.6 μm to 2.7 μm, PMSQ particle diameter of Example 2: 3.3 μm to 5.2 μm)
또한, 사용되는 촉매에 따라 주름 모양 PMSQ 입자의 직경이 변화하는 것을 알 수 있다. (실시예 1의 PMSQ 입자 직경: 2.6 ㎛ 내지 2.7 ㎛, 실시예 3의 PMSQ 입자 직경: 6.4 ㎛ 내지 7.6 ㎛, 실시예 4의 PMSQ 입자 직경: 8.6 ㎛ 내지 28.6 ㎛)In addition, it can be seen that the diameter of the corrugated PMSQ particles varies depending on the catalyst used. (PMSQ particle diameter of Example 1: 2.6 μm to 2.7 μm, PMSQ particle diameter of Example 3: 6.4 μm to 7.6 μm, PMSQ particle diameter of Example 4: 8.6 μm to 28.6 μm)
즉, 실란 원료의 첨가 비율을 조절하고, 첨가되는 촉매의 종류를 제어하는 것만으로 주름 깊이와 입자 크기를 제어할 수 있으며, 기능성 화장품, 난반사 필름 등의 다양한 물품에 적용 가능한 주름 모양 PMSQ 입자를 구현할 수 있다.That is, by controlling the addition ratio of the silane raw material and controlling the type of catalyst to be added, it is possible to control wrinkle depth and particle size, and to implement wrinkle-shaped PMSQ particles applicable to various articles such as functional cosmetics and diffuse reflection film. Can be.
도 3은 실시예 1의 주름 모양 PMSQ 입자 및 일반적인 PMSQ 입자의 XRD 결과이다.3 is an XRD result of the wrinkled PMSQ particles of Example 1 and general PMSQ particles.
도 3을 참조하면, 본 발명의 일 실시예에 따라 제조되는 주름 모양 PMSQ 입자는 기존의 PMSQ 입자와 비교하여 유사한 XRD 피크를 나타내는 것을 알 수 있다. 즉, 2 종 이상의 실란을 사용하여 PMSQ 입자를 구현할 수 있다.Referring to FIG. 3, it can be seen that the corrugated PMSQ particles prepared according to an embodiment of the present invention exhibit similar XRD peaks compared to the conventional PMSQ particles. That is, it is possible to implement PMSQ particles using two or more silanes.
도 4는 실시예 1의 주름 모양 PMSQ 입자의 FIB(Focused Ion Beam) 측정 결과이다.4 is a result of measuring the FIB (Focused Ion Beam) of the wrinkled PMSQ particles of Example 1.
도 4를 참조하면, FIB 측정 결과 실시예 1의 주름 모양 PMSQ 입자 내부가 완전히 채워져 있음을 알 수 있다. 이는, 내부의 기공을 통해 주름이 형성되는 것이 아님을 의미하며, 완전히 채워진 내부의 표면에 주름이 형성되는 것을 의미한다.Referring to FIG. 4, it can be seen that the inside of the wrinkled PMSQ particles of Example 1 was completely filled as a result of FIB measurement. This means that wrinkles are not formed through the pores inside, and wrinkles are formed on the completely filled interior surface.
도 5는 실시예 1의 주름 모양 PMSQ 입자를 포함하는 실시예의 PMSQ 파우더 및 일반적인 PMSQ 입자를 포함하는 비교예의 PMSQ 파우더의 혼용성을 비교한 이미지이다.5 is an image comparing the compatibility of the PMSQ powder of the comparative example containing the PMSQ powder and the general PMSQ particles of the embodiment containing the wrinkled PMSQ particles of Example 1.
도 5를 참조하면, 실시예의 PMSQ 파우더는 기존의 PMSQ 파우더와 비교하여 증류수(D.I Water base) 및 실리콘 오일(Silicone oil base)과의 혼용성이 우수한 것을 알 수 있다.Referring to FIG. 5, it can be seen that the PMSQ powder of the embodiment has excellent compatibility with distilled water (D.I Water base) and silicone oil (Silicone oil base) compared to the existing PMSQ powder.
도 6은 실시예 1의 주름 모양 PMSQ 입자 및 일반적인 PMSQ 입자의 SEM 이미지이다. 도 6을 참조하면, 실시예 1의 주름 모양 PMSQ 입자는 입자 표면이 주름진 것에 비해, 비교예의 PMSQ 입자는 표면 주름이 없는 것을 알 수 있다.6 is an SEM image of the wrinkled PMSQ particles of Example 1 and general PMSQ particles. Referring to FIG. 6, it can be seen that the corrugated PMSQ particles of Example 1 had no corrugated particles, whereas the PMSQ particles of the comparative example had no corrugated surfaces.
또한, 실시예 1의 주름 모양 PMSQ 입자 및 일반적인 PMSQ 입자를 이용하여 광학 시뮬레이션을 진행한 결과 주름 모양 PMSQ 입자는 일반적인 PMSQ 입자에 비해 빛의 난반사 효과가 뛰어남을 확인할 수 있었다.In addition, as a result of optical simulation using the pleated PMSQ particles of Example 1 and the general PMSQ particles, it was confirmed that the pleated PMSQ particles have superior light scattering effect compared to the general PMSQ particles.
즉, 본 발명의 일 실시예에 따른 PMSQ 파우더는 주름 모양 PMSQ 입자를 포함함으로써, 기존 실리콘 파우더와 비교하여 실리콘 오일 및 증류수와의 혼용성이 매우 우수하며, 광학 시뮬레이션 결과 기존 실리콘 파우더에 비해 빛의 난반사 효과가 뛰어나다. 또한, 엠보싱 효과로 피부 질감이 우수하여, 주름 은폐 효과가 뛰어나면서도 사용감이 불편하지 않은 기능성 화장품을 구현할 수 있다.That is, the PMSQ powder according to an embodiment of the present invention includes wrinkled PMSQ particles, so that it is very compatible with silicone oil and distilled water compared to the existing silicon powder, and the optical simulation results show that the light The diffuse reflection effect is excellent. In addition, the skin texture is excellent due to the embossing effect, so it is possible to implement a functional cosmetic product having an excellent wrinkle hiding effect and an uncomfortable feeling of use.
이상과 같이 실시예들이 비록 한정된 실시예와 도면에 의해 설명되었으나, 해당 기술분야에서 통상의 지식을 가진 자라면 상기의 기재로부터 다양한 수정 및 변형이 가능하다. 예를 들어, 설명된 기술들이 설명된 방법과 다른 순서로 수행되거나, 및/또는 설명된 구성요소들이 설명된 방법과 다른 형태로 결합 또는 조합되거나, 다른 구성요소 또는 균등물에 의하여 대치되거나 치환되더라도 적절한 결과가 달성될 수 있다. 그러므로, 다른 구현들, 다른 실시예들 및 특허청구범위와 균등한 것들도 후술하는 특허청구범위의 범위에 속한다.As described above, although the embodiments have been described by a limited embodiment and drawings, those skilled in the art can make various modifications and variations from the above description. For example, even if the described techniques are performed in a different order than the described method, and/or the described components are combined or combined in a different form from the described method, or replaced or replaced by another component or equivalent Appropriate results can be achieved. Therefore, other implementations, other embodiments, and equivalents to the claims are also within the scope of the following claims.

Claims (14)

  1. 유기용매에 선택된 촉매를 혼합하여 촉매 용액을 제조하는 단계;Preparing a catalyst solution by mixing a selected catalyst with an organic solvent;
    상기 촉매 용액에 서로 다른 2 종 이상의 실란을 첨가하여 반응 용액을 제조하는 단계; 및Preparing a reaction solution by adding two or more different silanes to the catalyst solution; And
    상기 반응 용액을 통해 표면에 주름이 형성된 PMSQ(폴리메틸실세스퀴옥세인, polymethylsilsesquioxane) 입자를 합성하는 단계;를 포함하는,Comprising the steps of synthesizing PMSQ (polymethylsilsesquioxane, polymethylsilsesquioxane) particles with wrinkles formed on the surface through the reaction solution;
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  2. 제1항에 있어서,According to claim 1,
    상기 서로 다른 2 종 이상의 실란은, 메틸트리에톡시실란 (methyltriethoxysilane), 메틸트리메톡시실란 (methyltrimethoxysilane), 디메틸디메톡시실란 (dimethyldimethoxysilane), 디메틸디에톡시실란 (dimethyldiethoxysilane), 노르말프로필트리메톡시실란 (N-propyltrimethoxysilane), 노르말프로필트리에톡시실란 (N-propyltriethoxysilane), 비닐트리메톡시실란 (Vinyltrimethoxysilane), 비닐트리에톡시시란 (Vinyltriethoxysilane), 페닐트리메톡시실란 (Phenyltrimethoxysilane), 페닐트리에톡시실란 (Phenyltriethoxysilane), 디페닐디메톡시실란 (Diphenyldimethoxysilane) 및 메틸페닐디메톡시실란 (Methylphenyldimethoxysilane)으로 이루어진 군으로부터 선택된 적어도 2 종을 포함하는 것인,The two or more different types of silanes include methyltriethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, and normalpropyl trimethoxysilane ( N-propyltrimethoxysilane, normal propyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane (Phenyltriethoxysilane), diphenyldimethoxysilane (Diphenyldimethoxysilane) and methylphenyldimethoxysilane (Methylphenyldimethoxysilane) to include at least two selected from the group consisting of,
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  3. 제1항에 있어서,According to claim 1,
    상기 서로 다른 2종 이상의 실란은, 메틸트리에톡시실란 (methyltriethoxysilane) 및 메틸트리메톡시실란(methyltrimethoxysilane)이고, The two or more different types of silanes are methyltriethoxysilane and methyltrimethoxysilane,
    상기 메틸트리에톡시실란 및 상기 메틸트리메톡시실란의 첨가 비율은 4 : 1 (몰) 내지 1 : 4 (몰)인 것인,The addition ratio of the methyl triethoxysilane and the methyl trimethoxysilane is from 4: 1 (mole) to 1: 4 (mole),
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  4. 제3항에 있어서,According to claim 3,
    상기 메틸트리메톡시실란의 첨가 비율이 올라갈수록 상기 주름 모양 PMSQ 입자의 주름 깊이의 높낮이차가 더욱 증가하는 것인,The higher the addition ratio of the methyltrimethoxysilane, the higher the difference in height of the wrinkle depth of the wrinkled PMSQ particles is,
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  5. 제3항에 있어서,According to claim 3,
    상기 메틸트리메톡시실란의 첨가 비율이 올라갈수록 상기 주름 모양 PMSQ 입자의 직경이 더욱 증가하는 것인,The more the methyl trimethoxysilane is added, the more the diameter of the corrugated PMSQ particles increases.
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  6. 제1항에 있어서,According to claim 1,
    상기 촉매 종류의 선택에 따라 상기 주름 모양 PMSQ 입자의 직경이 조절되는 것인,The diameter of the corrugated PMSQ particles is controlled according to the selection of the catalyst type,
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  7. 제1항에 있어서,According to claim 1,
    상기 촉매는, The catalyst,
    아미노프로필트리메톡시실란 (Aminopropyltrimethoxysilane), 트리에틸아민(Triethylamine), 수산화 암모늄(NH 4OH) 및 트리에탄올아민(Triethanolamine)으로 이루어진 군으로부터 선택되는 적어도 하나를 포함하는 것인,It comprises at least one selected from the group consisting of aminopropyltrimethoxysilane, triethylamine, ammonium hydroxide (NH 4 OH) and triethanolamine,
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  8. 제1항에 있어서,According to claim 1,
    상기 촉매는 아미노프로필트리메톡시실란(Aminopropyltrimethoxysilane)을 포함하고,The catalyst includes aminopropyltrimethoxysilane,
    상기 주름 모양 PMSQ 입자의 직경은 1 ㎛ 내지 6 ㎛인 것인,The diameter of the corrugated PMSQ particles is 1 μm to 6 μm,
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  9. 제1항에 있어서,According to claim 1,
    상기 촉매는 트리에틸아민(Triethylamine)을 포함하고,The catalyst includes triethylamine,
    상기 주름 모양 PMSQ 입자의 직경은 6 ㎛ 내지 8 ㎛인 것인,The diameter of the corrugated PMSQ particles is 6 μm to 8 μm,
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  10. 제1항에 있어서,According to claim 1,
    상기 촉매는 수산화 암모늄(NH 4OH)을 포함하고,The catalyst includes ammonium hydroxide (NH 4 OH),
    상기 주름 모양 PMSQ 입자의 직경은 8 ㎛ 내지 30 ㎛인 것인,The diameter of the corrugated PMSQ particles is 8 ㎛ to 30 ㎛,
    주름 모양 PMSQ 입자의 제조방법.Manufacturing method of corrugated PMSQ particles.
  11. 서로 다른 2 종 이상의 실란을 포함하고, 표면이 주름 형태인 주름 모양 PMSQ 입자를 포함하고,It contains two or more different types of silanes, and the surface contains corrugated PMSQ particles,
    상기 주름의 두께가 10 nm 내지 1000 nm이고, The thickness of the wrinkles is 10 nm to 1000 nm,
    상기 주름의 간격이 10 nm 내지 1000 nm인 것인,The spacing of the wrinkles is 10 nm to 1000 nm,
    PMSQ 파우더.PMSQ powder.
  12. 제11항에 있어서,The method of claim 11,
    상기 주름 모양 PMSQ 입자는,The wrinkled PMSQ particles,
    청구항 제1항 내지 제10항의 주름 모양 PMSQ 입자의 제조방법에 따라 제조된 것인,Claims 1 to 10 are manufactured according to the method of manufacturing the wrinkled PMSQ particles,
    PMSQ 파우더.PMSQ powder.
  13. 제11항의 PMSQ 파우더를 포함하는,Claim 11 comprising the PMSQ powder,
    기능성 화장품.functional cosmetics.
  14. 제11항의 PMSQ 파우더를 포함하는,Claim 11 comprising the PMSQ powder,
    난반사 필름. Diffuse reflection film.
PCT/KR2018/015306 2018-11-28 2018-12-05 Method for preparing wrinkle-shaped polymethylsilsesquioxane particles, and polymethylsilsesquioxane powder comprising polymethylsilsesquioxane particles prepared thereby WO2020111359A1 (en)

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Citations (5)

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Publication number Priority date Publication date Assignee Title
KR20050105567A (en) * 2004-04-30 2005-11-04 김영백 Method for manufacturing poly(silsesquioxane) spherical particle using alkoxysilane compound containing ammio group and poly(silsesquioxane) spherical particle
KR20070097461A (en) * 2004-12-27 2007-10-04 고니시가가꾸고오교가부시끼가이샤 Organic-solvent dispersion of fine polysilsesquioxane particle, process for producing the same, aqueous dispersion of fine polysilsesquioxane particle, and process for producing the same
US20080292863A1 (en) * 2007-02-16 2008-11-27 Shin Etsu Chemical Co., Ltd. Siloxane polymer, preparation method thereof, porous-film forming coating solution containing the polymer, porous film, and semiconductor device using the porous film
US20110200654A1 (en) * 2008-10-20 2011-08-18 Microcapsules Technologies Microcapsules having an envelope composed essentially of silsesquioxane homopolymers or copolymers
KR20180107182A (en) * 2016-02-01 2018-10-01 신에쓰 가가꾸 고교 가부시끼가이샤 Process for producing spherical polymethylphenylsilsequioxane particles

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JP4040362B2 (en) * 2002-05-20 2008-01-30 モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社 Method for producing spherical polymethylphenylsilsesquioxane fine particles

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20050105567A (en) * 2004-04-30 2005-11-04 김영백 Method for manufacturing poly(silsesquioxane) spherical particle using alkoxysilane compound containing ammio group and poly(silsesquioxane) spherical particle
KR20070097461A (en) * 2004-12-27 2007-10-04 고니시가가꾸고오교가부시끼가이샤 Organic-solvent dispersion of fine polysilsesquioxane particle, process for producing the same, aqueous dispersion of fine polysilsesquioxane particle, and process for producing the same
US20080292863A1 (en) * 2007-02-16 2008-11-27 Shin Etsu Chemical Co., Ltd. Siloxane polymer, preparation method thereof, porous-film forming coating solution containing the polymer, porous film, and semiconductor device using the porous film
US20110200654A1 (en) * 2008-10-20 2011-08-18 Microcapsules Technologies Microcapsules having an envelope composed essentially of silsesquioxane homopolymers or copolymers
KR20180107182A (en) * 2016-02-01 2018-10-01 신에쓰 가가꾸 고교 가부시끼가이샤 Process for producing spherical polymethylphenylsilsequioxane particles

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