JP7510250B2 - Porous composite powder for removing fine dust and its manufacturing method - Google Patents
Porous composite powder for removing fine dust and its manufacturing method Download PDFInfo
- Publication number
- JP7510250B2 JP7510250B2 JP2019145669A JP2019145669A JP7510250B2 JP 7510250 B2 JP7510250 B2 JP 7510250B2 JP 2019145669 A JP2019145669 A JP 2019145669A JP 2019145669 A JP2019145669 A JP 2019145669A JP 7510250 B2 JP7510250 B2 JP 7510250B2
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- JP
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- Prior art keywords
- composite powder
- porous composite
- fine dust
- removing fine
- magnetic particles
- Prior art date
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Description
本明細書には、細塵除去効果に優れる多孔性複合粉体及びその製造方法が開示される。 This specification discloses a porous composite powder with excellent fine dust removal properties and a method for producing the same.
ほこりが体内に蓄積されると、体内免疫力が低下し且つ心臓疾患や呼吸器疾患といった各種の疾患を誘発することがある。その上に気管支に狭窄を引き起こしたりもし、長期間吸い込むと喘息や肺疾患の有病率、早期死亡率を増加させる。 When dust accumulates in the body, it can weaken the body's immune system and induce various diseases such as heart disease and respiratory disease. It can also cause bronchial narrowing, and if inhaled for a long period of time, it can increase the prevalence of asthma and lung disease, as well as early mortality.
肌はほこりと直接的に触れる身体の最も表側であって、有機体と環境との間のバリアの役割を果たし、汚染への露出が頻繁になると、かかるバリア機能が低下する。特に、細塵は毛穴の20分の1と小さいため、肌中に容易に浸透することができる。実際のところ、細塵のような大気汚染物質は、肌健康に深刻な影響を与えると知られている。短期的には早期老化、水分不足、小じわとしわを増加させ、長期的には取り戻せない肌損傷によって肌が環境的要素から身を保護する機能を喪失するとともに、皮膚癌のような深刻な病気を誘発させることがある。 The skin is the outermost part of the body that comes into direct contact with dust and acts as a barrier between the organism and the environment, and frequent exposure to pollution weakens this barrier function. Fine dust, in particular, is 20 times smaller than a hair follicle and can easily penetrate the skin. In fact, air pollutants such as fine dust are known to have serious effects on skin health. In the short term, they can cause premature aging, dehydration, and increased fine lines and wrinkles, and in the long term, they can cause irreversible skin damage that causes the skin to lose its ability to protect itself from environmental elements and can even lead to serious diseases such as skin cancer.
特に、肌の上に堆積しているほこりは、既存の各種のクレンザーを利用してその多くを除去することができるが、毛穴の中に浸透している細塵の除去は容易ではない。よって、毛穴の中に残存している肌に有害で且つ人体に致命的な障害を引き起こす有害物質である細塵を効果的に除去するための機能性複合粉体構造体に関する研究が必要である。また、毛穴の中で作用する原料であることから、刺激フリーで且つ安全な生体親和性素材の選択が重要である。 In particular, while most of the dust that accumulates on the skin can be removed using various existing cleansers, it is not easy to remove the fine dust that has penetrated into the pores. Therefore, research is needed on functional composite powder structures that can effectively remove the fine dust that remains in the pores and is harmful to the skin and can cause fatal damage to the human body. In addition, since the raw material acts inside the pores, it is important to select a biocompatible material that is non-irritating and safe.
一側面において、本発明の目的は、多孔性複合粉体を用いて、肌に付着している細塵が含まれた皮脂などを効果的に多孔性複合粉体に吸引させることである。 In one aspect, the object of the present invention is to use a porous composite powder to effectively absorb sebum and other particles that contain fine dust adhering to the skin into the porous composite powder.
他の側面において、本発明の目的は、磁性粒子を含む多孔性複合粉体とマグネチックアプリケータを用いて、肌と毛穴の中に残存している細塵を効果的に除去することである。 In another aspect, the object of the present invention is to effectively remove fine dust particles remaining on the skin and in pores using a porous composite powder containing magnetic particles and a magnetic applicator.
他の側面において、本発明の目的は、簡便な工程で磁性粒子が均一に含浸された細塵除去用多孔性複合粉体を製造することである。 In another aspect, the object of the present invention is to produce a porous composite powder for removing fine dust, which is uniformly impregnated with magnetic particles, by a simple process.
一側面において、本発明は、高分子、及び前記高分子に含浸された磁性粒子を含む細塵除去用多孔性複合粉体を提供する。 In one aspect, the present invention provides a porous composite powder for removing fine dust, comprising a polymer and magnetic particles impregnated in the polymer.
他の一側面において、本発明は、前述した多孔性複合粉体を含む組成物を提供する。 In another aspect, the present invention provides a composition comprising the porous composite powder described above.
他の一側面において、本発明は、前述した組成物を肌の上に塗布する段階、及びマグネチックアプリケータを用いて前記多孔性複合粉体を肌から脱着する段階を含む細塵除去方法を提供する。 In another aspect, the present invention provides a method for removing fine dust, comprising the steps of applying the composition described above onto the skin and detaching the porous composite powder from the skin using a magnetic applicator.
他の一側面において、本発明は、前述した多孔性複合粉体の製造方法であって、高分子を含む溶液を製造する段階と、磁性粒子を前記高分子を含む溶液に分散させる段階、及び前記磁性粒子が分散された溶液を噴霧乾燥する段階と、を含む細塵除去用多孔性複合粉体の製造方法を提供する。 In another aspect, the present invention provides a method for producing the porous composite powder for removing fine dust, comprising the steps of preparing a solution containing a polymer, dispersing magnetic particles in the solution containing the polymer, and spray-drying the solution in which the magnetic particles are dispersed.
一側面において、本発明に係る細塵除去用多孔性複合粉体は、多孔性を有する高分子に磁性粒子を均一に含浸させ、細塵が含まれた皮脂を気孔内部に吸いこませた後、マグネチックアプリケータを用いて肌から容易に脱着させることで肌と毛穴の中に残存している細塵を効果的に除去する。 In one aspect, the porous composite powder for removing fine dust according to the present invention is made by uniformly impregnating a porous polymer with magnetic particles, sucking the sebum containing fine dust into the pores, and then easily detaching it from the skin using a magnetic applicator, thereby effectively removing fine dust remaining on the skin and in the pores.
用語の定義
本明細書において「磁性粒子」とは、強磁性(Ferromagnetic、Fe、Ni、Coなど)、フェリ磁性(Ferrimagnetic、Fe2O3、MnFe2O4、BAO6Fe2O3など)、常磁性(Paramagnetic、Al、Ti、Cu合金など)、超常磁性(superparamagnetic、Fe3O4など)など、磁性を持つ粒子であれば磁性の程度や種類に制限されることなく、いずれも含む。また、前記磁性粒子は含浸可能なものであってよい。
Definition of Terms In this specification, the term "magnetic particles" refers to any particles having magnetism, such as ferromagnetic (Ferromagnetic, Fe, Ni, Co, etc.), ferrimagnetic (Ferrimagnetic, Fe2O3 , MnFe2O4 , BAO6Fe2O3 , etc.), paramagnetic (Paramagnetic, Al, Ti, Cu alloy, etc.), superparamagnetic (Superparamagnetic, Fe3O4 , etc.), etc., without being limited by the degree or type of magnetism. In addition, the magnetic particles may be impregnable.
本明細書において「ほこり」とは、大気中に混ざっている微粒子の総称であって、通常、10mm以下の粒径を有する浮遊物質を意味する。特に、粒径が10μm以下のものを細塵、2.5μm以下のものを超細塵、0.1μm以下のものを極細塵とも言う。ここで、粒径とは、各細塵の粒径の平均値を意味してよい。ほこりは、砂、土、及び花粉といった自然から由来した物質または炭素、炭素燃焼物、金属塩及び重金属といった産業工程から由来した物質などを含む物質である。ほこりの形態は、ヒューム(fume)、ミスト(mist)、煙、蒸気、または煙霧であってよい。 In this specification, "dust" is a general term for fine particles mixed in the air, and generally refers to suspended matter having a particle size of 10 mm or less. In particular, particles having a particle size of 10 μm or less are called fine dust, particles having a particle size of 2.5 μm or less are called ultrafine dust, and particles having a particle size of 0.1 μm or less are called extremely fine dust. Here, particle size may refer to the average particle size of each particle of fine dust. Dust is a material that includes natural substances such as sand, soil, and pollen, or substances derived from industrial processes such as carbon, carbon combustion products, metal salts, and heavy metals. Dust may take the form of fumes, mist, smoke, steam, or smoke.
本明細書において「粒径」とは、粒子の直径を意味し、定義された粒径の範囲はそれぞれの単一粒子の直径の範囲を意味する。 In this specification, "particle size" refers to the diameter of a particle, and the defined particle size range refers to the range of diameters of each individual particle.
本明細書において、ある部分がある構成要素を「含む」とするとき、これは、特に逆の記載がない限り、他の構成要素を除くのではなく、他の構成要素をさらに含んでよいことを意味する。 In this specification, when a part "contains" a certain component, this does not mean to exclude other components, but may further include other components, unless otherwise specified.
例示的な具現例の説明
以下、本発明について詳しく説明する。
DETAILED DESCRIPTION OF ILLUSTRATIVE EMBODIMENTS The present invention will now be described in detail.
細塵除去用多孔性複合粉体
本発明の例示的な具現例では、高分子、及び前記高分子に含浸された磁性粒子を含む細塵除去用多孔性複合粉体を提供する。
Porous Composite Powder for Removing Fine Dust According to an exemplary embodiment of the present invention, there is provided a porous composite powder for removing fine dust, comprising a polymer and magnetic particles impregnated in the polymer.
従来、多孔性シリカや多孔性高分子粒子を用いて毛穴の中に存在する細塵を皮脂と一緒に吸いこむことは可能であるが、一度毛穴の中に入った多孔性粒子を外部に再び取り出すことは至難であるということが致命的な問題点である。 Conventionally, it has been possible to use porous silica or porous polymer particles to suck up fine dust particles present in pores together with sebum, but a fatal problem is that once porous particles have entered the pores, it is extremely difficult to remove them again.
これを克服するために、本発明者らは、多孔性高分子中に磁性を帯びる磁性粒子を均一に含浸して、毛穴の中に浸透して皮脂と混ざっている細塵を毛細管現象によって吸いこんだ後、マグネチックアプリケータを用いて前記多孔性複合粉体を毛穴の外に容易に取り出して肌から安全に脱着させるための細塵除去用多孔性複合粉体を発明した(図8)。 To overcome this, the inventors invented a porous composite powder for removing fine dust, which is made by uniformly impregnating a porous polymer with magnetic particles, and which penetrates into the pores and sucks in fine dust mixed with sebum through capillary action, and then uses a magnetic applicator to easily remove the porous composite powder from the pores and safely detach it from the skin (Figure 8).
具体的に、噴霧乾燥技術を導入すれば、多孔性高分子中に磁性粒子が均一に含浸された複合粉体を単一工程で製造可能であり、当該高分子の場合、肌親和性を極大化させるために生分解性高分子が適用可能であることが本技術の大きな長所である(図7)。 Specifically, by using spray drying technology, it is possible to produce a composite powder in which magnetic particles are uniformly impregnated into a porous polymer in a single process. In the case of the polymer, a biodegradable polymer can be used to maximize skin affinity, which is a major advantage of this technology (Figure 7).
一具現例において、前記高分子は、ポリメチルメタクリレート(PMMA)、ポリスチレン(PS)、ポリビニルピロリドン(PVP)、ポリカプロラクトン(PCL)、ポリ乳酸(PLA)、及び乳酸・グリコール酸共重合体(PLGA)からなる群より選ばれる1以上であってよく、ジクロロメタン、エタノール、アセトンなどに溶解されるものであれば特に制限されない。 In one embodiment, the polymer may be one or more selected from the group consisting of polymethyl methacrylate (PMMA), polystyrene (PS), polyvinylpyrrolidone (PVP), polycaprolactone (PCL), polylactic acid (PLA), and lactic acid-glycolic acid copolymer (PLGA), and is not particularly limited as long as it is soluble in dichloromethane, ethanol, acetone, etc.
一具現例において、前記高分子は生分解性高分子であってよく、ポリカプロラクトン(PCL)、ポリ乳酸(PLA)、及び乳酸・グリコール酸共重合体(PLGA)からなる群より選ばれる1以上であってよく、好ましくは、乳酸・グリコール酸共重合体(PLGA)であってよい。本発明では、生分解性高分子を適用することで、プラスチックマイクロビーズのイシューを排除するとともに、毛穴の中で作用するにもかかわらず肌に対する生体親和性を向上させることができる。 In one embodiment, the polymer may be a biodegradable polymer, and may be one or more selected from the group consisting of polycaprolactone (PCL), polylactic acid (PLA), and polylactic acid-glycolic acid copolymer (PLGA), and may be preferably polylactic acid-glycolic acid copolymer (PLGA). In the present invention, by applying a biodegradable polymer, the issues of plastic microbeads can be eliminated and biocompatibility with the skin can be improved despite acting inside pores.
一具現例において、前記磁性粒子は、Fe、Ni、Co、MnFe2O4、BaO・6Fe2O3、Alの合金、Tiの合金、Cuの合金、及び酸化鉄からなる群より選ばれる1以上であってよく、好ましくは、Fe3O4であってよい。 In one embodiment, the magnetic particles may be one or more selected from the group consisting of Fe , Ni , Co, MnFe2O4 , BaO.6Fe2O3 , an alloy of Al, an alloy of Ti, an alloy of Cu, and iron oxide, and may be preferably Fe3O4 .
一具現例において、前記多孔性複合粉体の全重量を基準に前記磁性粒子の含浸の割合は、50~90重量%の範囲であってよく、例えば、55重量%以上、60重量%以上、65重量%以上または70重量%以上であってよく、且つ88重量%以下、86重量%以下、84重量%以下、82重量%以下または80重量%以下であってよい。前記含浸の割合が50重量%未満であると、磁性が弱いため毛穴から皮脂を吸いこんだ多孔性複合粉体を取り除き難いことがあり、90重量%を超えると、磁性は増加するものの、皮脂吸油量が減少することがある。 In one embodiment, the impregnation ratio of the magnetic particles based on the total weight of the porous composite powder may be in the range of 50 to 90% by weight, for example, 55% by weight or more, 60% by weight or more, 65% by weight or more, or 70% by weight or more, and 88% by weight or less, 86% by weight or less, 84% by weight or less, 82% by weight or less, or 80% by weight or less. If the impregnation ratio is less than 50% by weight, the porous composite powder that has absorbed sebum from the pores may be difficult to remove due to weak magnetism, and if it exceeds 90% by weight, the magnetism increases but the sebum absorption may decrease.
一具現例において、前記多孔性複合粉体の粒径は、10~100μmの範囲であってよく、例えば、15μm以上、20μm以上、25μm以上または30μm以上であってよく、且つ95μm以下、85μm以下、80μm以下、75μm以下、70μm以下、65μm以下、60μm以下、55μm以下または50μm以下であってよい。前記粒径が10μm未満であると、肌上の細塵が含まれた皮脂などを十分に吸いこみ難いことがあり、前記粒径が100μmを超えると、実際に肌上への塗布の際に粒子感または異物感が感じられることがある。 In one embodiment, the particle size of the porous composite powder may be in the range of 10 to 100 μm, for example, 15 μm or more, 20 μm or more, 25 μm or more, or 30 μm or more, and may be 95 μm or less, 85 μm or less, 80 μm or less, 75 μm or less, 70 μm or less, 65 μm or less, 60 μm or less, 55 μm or less, or 50 μm or less. If the particle size is less than 10 μm, it may be difficult to sufficiently absorb sebum containing fine dust on the skin, and if the particle size exceeds 100 μm, a grainy or foreign body feeling may be felt when actually applied to the skin.
一具現例において、前記多孔性複合粉体の気孔の直径は、100nm~10μmであってよく、例えば、150nm以上、200nm以上、250nm以上、300nm以上、350nm以上、400nm以上、450nm以上、または500nm以上であってよく、且つ9μm以下、8μm以下、7μm以下、6μm以下、5μm以下、4μm以下、3μm以下、2μm以下、または1μm以下であってよい。前記気孔の直径が100nm未満であると、気孔の内部に細塵が含まれた皮脂を吸いこみ難いことがあり、10μmを超えると、機械的強度が低下して粒子が砕け易くなる可能性が高い。 In one embodiment, the pore diameter of the porous composite powder may be 100 nm to 10 μm, for example, 150 nm or more, 200 nm or more, 250 nm or more, 300 nm or more, 350 nm or more, 400 nm or more, 450 nm or more, or 500 nm or more, and 9 μm or less, 8 μm or less, 7 μm or less, 6 μm or less, 5 μm or less, 4 μm or less, 3 μm or less, 2 μm or less, or 1 μm or less. If the pore diameter is less than 100 nm, it may be difficult to absorb sebum containing fine dust inside the pores, and if it exceeds 10 μm, there is a high possibility that the mechanical strength will decrease and the particles will be easily broken.
一具現例において、前記多孔性複合粉体の平均気孔直径(Average Pore Diameter、4V/A)は、0.01~2μmであってよく、例えば、0.05μm以上、0.1μm以上、0.2μm以上、または0.3μm以上であってよく、且つ1.7μm以下、1.5μm以下、1.3μm以下、1.1μm以下、0.9μm以下、0.8μm以下、0.7μm以下、0.6μm以下、0.5μm以下、または0.4μm以下であってよい。 In one embodiment, the average pore diameter (4V/A) of the porous composite powder may be 0.01 to 2 μm, for example, 0.05 μm or more, 0.1 μm or more, 0.2 μm or more, or 0.3 μm or more, and 1.7 μm or less, 1.5 μm or less, 1.3 μm or less, 1.1 μm or less, 0.9 μm or less, 0.8 μm or less, 0.7 μm or less, 0.6 μm or less, 0.5 μm or less, or 0.4 μm or less.
一具現例において、前記多孔性複合粉体の孔隙率(porosity)は30~80%であってよく、例えば、35%以上、40%以上、45%以上、50%以上、55%以上、60%以上でであってよく、且つ75%以下、70%以下、または65%以下であってよい。前記孔隙率は、実際に細塵を含む皮脂を吸油することができる気孔の全体割合を意味しており、30%未満であると、細塵除去効果が微々たるものとなることがあり、80%を超えると、機械的強度が低下して粒子が砕け易くなる可能性が高い。 In one embodiment, the porosity of the porous composite powder may be 30-80%, for example, 35% or more, 40% or more, 45% or more, 50% or more, 55% or more, 60% or more, and 75% or less, 70% or less, or 65% or less. The porosity refers to the total ratio of pores that can actually absorb sebum including fine dust, and if it is less than 30%, the fine dust removal effect may be negligible, and if it exceeds 80%, the mechanical strength may decrease and the particles may be easily broken.
一具現例において、前記多孔性複合粉体の磁性の強さは、磁力計(Magnetometer)で測定した値が30~70emu/gであってよく、例えば、35emu/g以上、40emu/g以上、45emu/g以上、または50emu/g以上であってよく、且つ65emu/g以下、60emu/g以下、または55emu/g以下であってよい。前記磁性の強さが30emu/g未満であると、肌から細塵を含む皮脂を吸いこんだ本発明に係る多孔性複合粉体を除去し難いことがあり、70emu/gを超えると、マグネチックアプリケータからの前記複合粉体の取り外しが至難となることがある。 In one embodiment, the magnetic strength of the porous composite powder may be 30 to 70 emu/g as measured by a magnetometer, for example, 35 emu/g or more, 40 emu/g or more, 45 emu/g or more, or 50 emu/g or more, and 65 emu/g or less, 60 emu/g or less, or 55 emu/g or less. If the magnetic strength is less than 30 emu/g, it may be difficult to remove the porous composite powder according to the present invention that has absorbed sebum including fine dust from the skin, and if it exceeds 70 emu/g, it may be extremely difficult to remove the composite powder from the magnetic applicator.
一具現例において、前記多孔性複合粉体は、粒径が2.5μm以下の細塵を除去することができ、例えば、2μm以下、1.5μm以下、または1μm以下の細塵も除去することができる。本発明に係る多孔性複合粉体は、粒径の小さい細塵が毛穴の中に浸透しても、毛穴の中に皮脂と混ざっている細塵を毛細管現象にて吸いこみ、後述するマグネチックアプリケータを用いて毛穴の外へと容易に取り出すことができるので、肌上の有害物質を簡易に除去することができる。 In one embodiment, the porous composite powder can remove fine dust particles having a particle size of 2.5 μm or less, for example, fine dust particles having a particle size of 2 μm or less, 1.5 μm or less, or 1 μm or less. Even if fine dust particles having a small particle size penetrate into the pores, the porous composite powder according to the present invention can easily remove harmful substances from the skin by sucking in the fine dust particles mixed with sebum in the pores through capillary action and easily removing the fine dust particles from the pores using a magnetic applicator described below.
本発明の例示的な具現例では、前述した多孔性複合粉体を含む細塵除去用組成物を提供する。 In an exemplary embodiment of the present invention, a composition for removing fine dust is provided that includes the porous composite powder described above.
一具現例において、前記組成物の総重量を基準にして前記多孔性複合粉体の含量は、30~70重量%の範囲であってよく、例えば、35重量%以上、40重量%以上、45重量%以上、または50重量%以上であってよく、且つ65重量%以下、60重量%以下、または55重量%であってよい。前記含量が30重量%未満であると、細塵除去効果が微々たるものとなることがあり、70重量%を超えると、異物感が感じられることがあり、肌に有害となることがある。 In one embodiment, the content of the porous composite powder may be in the range of 30 to 70 wt %, for example, 35 wt % or more, 40 wt % or more, 45 wt % or more, or 50 wt % or more, and 65 wt % or less, 60 wt % or less, or 55 wt % or less, based on the total weight of the composition. If the content is less than 30 wt %, the dust removal effect may be insignificant, and if it exceeds 70 wt %, a foreign body sensation may be felt and may be harmful to the skin.
一具現例において、前記組成物は化粧料組成物であってよく、化粧料組成物の外形は化粧品学または皮膚科学的に許容可能な媒質または基剤を含有する。これは局所適用に適合したあらゆる剤形で、例えば、溶液、ゲル、固体、練り無水生成物、水相に油相を分散させて得たエマルジョン、懸濁液、マイクロエマルジョン、マイクロカプセル、微細果粒球若しくはイオン型(リポソーム)及び非イオン型の小胞分散剤の形態で、またはクリーム、スキン、ローション、パウダー、軟膏、スプレー若しくはコンシールスティックの形態で提供されてよい。これらの組成物は、当該分野の通常的な方法によって製造されてよい。また、本発明に係る組成物は、泡沫(foam)の形態で、または圧縮された推進剤をさらに含有したエアロゾル組成物の形態でも用いられてよい。 In one embodiment, the composition may be a cosmetic composition, the cosmetic composition comprising a cosmetically or dermatologically acceptable medium or base. It may be provided in any formulation suitable for topical application, for example in the form of a solution, gel, solid, paste-based anhydrous product, emulsion obtained by dispersing an oily phase in an aqueous phase, suspension, microemulsion, microcapsule, microgranule or vesicular dispersion of ionic (liposome) and non-ionic type, or in the form of a cream, skin, lotion, powder, ointment, spray or conceal stick. These compositions may be prepared by conventional methods in the art. The composition according to the present invention may also be used in the form of a foam or in the form of an aerosol composition further containing a compressed propellant.
本発明の一実施例に係る前記化粧料組成物は、その剤形において特に限定されるところがなく、例えば、柔軟化粧水、収斂化粧水、栄養化粧水、栄養クリーム、マッサージクリーム、エッセンス、アイクリーム、アイエッセンス、クレンジングクリーム、クレンジングフォーム、クレンジングウォーター、前記化粧料組成物を含むクレンジングティッシュ、パック、パウダー、ボディローション、ボディクリーム、ボディオイル及びボディエッセンスなどの化粧品に剤形化されてよい。 The cosmetic composition according to one embodiment of the present invention is not particularly limited in its formulation, and may be formulated into cosmetics such as, for example, softening lotion, astringent lotion, nourishing lotion, nourishing cream, massage cream, essence, eye cream, eye essence, cleansing cream, cleansing foam, cleansing water, cleansing tissue containing the cosmetic composition, pack, powder, body lotion, body cream, body oil, and body essence.
本発明の剤形がペースト、クリームまたはゲルである場合には、担体成分として、動物繊維、植物繊維、ワックス、パラフィン、澱粉、トラガカント、セルロース誘導体、ポリエチレングリコール、シリコン、ベントナイト、シリカ、タルクまたは酸化亜鉛等が用いられてよい。 When the dosage form of the present invention is a paste, cream or gel, the carrier component may be animal fiber, vegetable fiber, wax, paraffin, starch, tragacanth, cellulose derivatives, polyethylene glycol, silicone, bentonite, silica, talc or zinc oxide.
本発明の剤形がパウダーまたはスプレーである場合には、担体成分として、ラクトース、タルク、シリカ、アルミニウムヒドロキシド、カルシウムシリケートまたはポリアミドパウダーが用いられてよく、特に、スプレーである場合には、さらにクロロフルオロヒドロカーボン、プロパン/ブタンまたはジメチルエーテルといった推進体を含んでよい。 When the dosage form of the present invention is a powder or a spray, lactose, talc, silica, aluminum hydroxide, calcium silicate or polyamide powder may be used as a carrier component, and particularly when the dosage form is a spray, it may further contain a propellant such as chlorofluorohydrocarbon, propane/butane or dimethyl ether.
本発明の剤形が溶液または乳濁液である場合には、担体成分として、溶媒、溶媒和剤または乳濁化剤が用いられてよく、例えば、水、エタノール、イソプロパノール、エチルカーボネート、エチルアセテート、ベンジルアルコール、ベンジルベンゾエート、プロピレングリコール、1,3‐ブチルグリコールオイル、グリセロール脂肪族エステル、ポリエチレングリコールまたはソルビタンの脂肪酸エステルがある。 When the dosage form of the present invention is a solution or emulsion, a solvent, solvating agent or emulsifier may be used as a carrier component, such as water, ethanol, isopropanol, ethyl carbonate, ethyl acetate, benzyl alcohol, benzyl benzoate, propylene glycol, 1,3-butyl glycol oil, glycerol aliphatic esters, polyethylene glycol or fatty acid esters of sorbitan.
本発明の剤形が懸濁液である場合には、担体成分として、水、エタノールまたはプロピレングリコールといった液状希釈剤、エトキシル化イソステアリルアルコール、ポリオキシエチレンソルビトールエステル及びポリオキシエチレンソルビタンエステルといった懸濁剤、微小結晶性セルロース、アルミニウムメタヒドロキシド、ベントナイト、アガーまたはトラガカントなどが用いられてよい。 When the dosage form of the present invention is a suspension, the carrier component may be a liquid diluent such as water, ethanol or propylene glycol, a suspending agent such as ethoxylated isostearyl alcohol, polyoxyethylene sorbitol ester and polyoxyethylene sorbitan ester, microcrystalline cellulose, aluminum metahydroxide, bentonite, agar or tragacanth.
本発明の剤形が界面活性剤含有クレンジングである場合には、担体成分として、脂肪族アルコールソルフェート、脂肪族アルコールエーテルソルフェート、スルホコハク酸モノエステル、イセチオネート、イミダゾリニウム誘導体、メチルタウレート、サルコシネート、脂肪酸アミドエーテルソルフェート、アルキルアミドベタイン、脂肪族アルコール、脂肪酸グリセリド、脂肪酸ジエタノールアミド、植物性油、リノリン誘導体またはエトキシル化グリセロール脂肪酸エステルなどが用いられてよい。 When the dosage form of the present invention is a surfactant-containing cleanser, the carrier component may be fatty alcohol sorbate, fatty alcohol ether sorbate, sulfosuccinic acid monoester, isethionate, imidazolinium derivative, methyl taurate, sarcosinate, fatty acid amide ether sorbate, alkylamidobetaine, fatty alcohol, fatty acid glyceride, fatty acid diethanolamide, vegetable oil, linolin derivative, or ethoxylated glycerol fatty acid ester.
本発明の一実施例に係る化粧料組成物には、前記多孔性複合粉体以外に、機能性添加物及び一般的な化粧料組成物に含まれる成分がさらに含まれてよい。前記機能性添加物としては、水溶性ビタミン、油溶性ビタミン、高分子ペプチド、高分子多糖、スフィンゴ脂質及び海藻エキスからなる群より選ばれた成分を含んでよい。 The cosmetic composition according to one embodiment of the present invention may further include functional additives and ingredients contained in general cosmetic compositions in addition to the porous composite powder. The functional additives may include ingredients selected from the group consisting of water-soluble vitamins, oil-soluble vitamins, polymeric peptides, polymeric polysaccharides, sphingolipids, and seaweed extracts.
本発明に係る化粧料組成物には、さらに、前記機能性添加物とともに、必要に応じて、一般的な化粧料組成物に含まれる成分を配合してもよい。その他に含まれる配合成分としては、油脂成分、保湿剤、エモリエント剤、界面活性剤、有機及び無機顔料、有機粉体、紫外線吸収剤、防腐剤、殺菌剤、酸化防止剤、植物抽出物、pH調整剤、アルコール、色素、香料、血行促進剤、冷感剤、制汗剤、精製水などが挙げられる。 The cosmetic composition according to the present invention may further contain, in addition to the functional additives, ingredients contained in general cosmetic compositions, if necessary. Other ingredients that may be contained include oils and fats, moisturizers, emollients, surfactants, organic and inorganic pigments, organic powders, UV absorbers, preservatives, bactericides, antioxidants, plant extracts, pH adjusters, alcohol, colorants, fragrances, blood circulation promoters, cooling agents, antiperspirants, purified water, etc.
本発明の例示的な具現例では、前述した組成物を肌の上に塗布する段階;及びマグネチックアプリケータを用いて前記多孔性複合粉体を肌から脱着する段階;を含む細塵除去方法を提供する。 In an exemplary embodiment of the present invention, a method for removing fine dust is provided, which includes the steps of applying the above-described composition onto the skin and detaching the porous composite powder from the skin using a magnetic applicator.
前記マグネチックアプリケータは、先がちびたさじ状の形態を有していてよいが、これに制限されない。また、ネオジミウム磁石を用いてヘッド部分の底面の表面に2000~4000Gの磁性を呈し得るようにすることができるが、これに制限されない。 The magnetic applicator may have a spoon-like shape with a short tip, but is not limited to this. In addition, a neodymium magnet may be used so that the surface of the bottom of the head portion can exhibit a magnetic field of 2000 to 4000 G, but is not limited to this.
細塵除去用多孔性複合粉体の製造方法
本発明の例示的な具現例では、前述した多孔性複合粉体の製造方法であって、高分子を含む溶液を製造する段階;磁性粒子を前記高分子を含む溶液に分散させる段階;及び前記磁性粒子が分散された溶液を噴霧乾燥する段階;を含む細塵除去用多孔性複合粉体の製造方法を提供する。
A method for manufacturing a porous composite powder for removing fine dust In an exemplary embodiment of the present invention, a method for manufacturing the porous composite powder described above is provided, which includes the steps of: preparing a solution containing a polymer; dispersing magnetic particles in the solution containing the polymer; and spray-drying the solution in which the magnetic particles are dispersed.
具体的に、図1を参照すると、前記高分子をDCMのような有機溶媒に溶解して高分子を含む溶液を準備し、前記溶液に磁性粒子を入れてこれをホモジナイザー(Homogenizer)を用いて分散させることができる。その後、前記磁性粒子が分散された溶液をノズルを介して噴霧乾燥して細塵除去用多孔性複合粉体を製造することができる。 Specifically, referring to FIG. 1, the polymer is dissolved in an organic solvent such as DCM to prepare a solution containing the polymer, and magnetic particles are added to the solution, which can then be dispersed using a homogenizer. The solution in which the magnetic particles are dispersed can then be spray-dried through a nozzle to produce a porous composite powder for removing fine dust.
このように噴霧乾燥技術を用いて高分子の内部に磁性粒子が均一に含浸された多孔性複合粉体を単一の工程で簡易に製造することができる。 In this way, using spray drying technology, it is possible to easily produce porous composite powder in which magnetic particles are uniformly impregnated inside a polymer in a single process.
このとき、噴霧乾燥器の内部湿度は30%以上に保持し、内部温度は室温を保持してよく、供給量(Feed rate):20%、吸引装置(Aspirator):70%、20atmの条件で噴霧乾燥してよい。 At this time, the internal humidity of the spray dryer may be maintained at 30% or more, the internal temperature may be maintained at room temperature, and spray drying may be performed under the following conditions: feed rate: 20%, aspirator: 70%, 20 atm.
一具現例において、前記噴霧乾燥の際、ポンプに流入される前の容器で前記磁性粒子が分散された溶液を撹拌してよく、これにより、噴霧乾燥の前に磁性粒子が沈殿することを防止することができる。 In one embodiment, during the spray drying, the solution in which the magnetic particles are dispersed may be stirred in a container before being pumped, thereby preventing the magnetic particles from settling before spray drying.
一具現例において、前記高分子を含む溶液の溶媒は、ジクロロメタン(Dichloromethane anhydrous)、エタノール及びアセトンからなる群より選ばれる1以上であってよく、好ましくは、ジクロロメタンであってよい。 In one embodiment, the solvent of the solution containing the polymer may be one or more selected from the group consisting of dichloromethane anhydrous, ethanol, and acetone, and may be preferably dichloromethane.
一具現例において、前記噴霧乾燥段階の後に、メタノール洗浄及びトレー乾燥する段階;をさらに含んでいてよく、これにより、残存溶媒を完全に除去した多孔性複合粉体を得ることができる。 In one embodiment, the method may further include a methanol washing and tray drying step after the spray drying step, thereby obtaining a porous composite powder from which the remaining solvent has been completely removed.
以下、下記の実施例により本発明をより具体的に説明する。なお、下記の実施例は本発明についての理解を助けるために例示の目的から提供したものであるに過ぎず、本発明の範疇及び範囲がこれに限定されるものではない。 The present invention will now be described in more detail with reference to the following examples. Note that the following examples are provided merely for illustrative purposes to aid in understanding the present invention, and are not intended to limit the scope of the present invention.
実施例 - 細塵用多孔性複合粉体の製造
先ず、磁性粒子(酸化鉄、大東化成工業社製)、乳酸・グリコール酸共重合体(lactic acid/glycolic acid copolymer、PLGA、GALACTIC社製)、ジクロロメタン(DCM、Dichloromethane anhydrous、Sigma-Aldrich社製、純度>99.8%)を準備し、下記のように磁性粒子が含浸された乳酸・グリコール酸共重合体(PLGA)複合粉体(以下、AP球)を製造した。
Example - Preparation of porous composite powder for fine dust First, magnetic particles (iron oxide, manufactured by Daito Chemical Industry Co., Ltd.), lactic acid/glycolic acid copolymer (PLGA, manufactured by Galactic Corporation), and dichloromethane anhydrous (DCM, manufactured by Sigma-Aldrich, purity >99.8%) were prepared, and lactic acid/glycolic acid copolymer (PLGA) composite powder impregnated with magnetic particles (hereinafter referred to as AP spheres) was prepared as follows.
1)PLGA 40gを溶媒DCM 1Lに溶解させた。
2)磁性粒子40gをPLGA溶液に入れた後、ホモジナイザー(Homogenizer)を用いて分散させた。
3)磁性粒子が分散されたPLGA溶液を本出願人自社製作の噴霧乾燥器を用いて噴霧乾燥した(図1参照)。
4)噴霧乾燥器の内部湿度は30%以上に保持し、内部温度は室温を保持した。
5)供給率(Feed rate):20%、吸引装置(Aspirator):70%、20atmの条件で噴霧乾燥した。磁性粒子が分散されたPLGA溶液は噴霧乾燥中に持続的に撹拌機にて撹拌した。
6)噴霧乾燥された磁性粒子/PLGA複合粉体を十分に洗浄した後、乾燥し、残存溶媒を完全に除去した後に収得した。
1) 40 g of PLGA was dissolved in 1 L of DCM solvent.
2) 40 g of magnetic particles were added to the PLGA solution and then dispersed using a homogenizer.
3) The PLGA solution in which the magnetic particles were dispersed was spray-dried using a spray dryer manufactured by the applicant (see FIG. 1).
4) The internal humidity of the spray dryer was maintained at 30% or higher, and the internal temperature was maintained at room temperature.
5) The mixture was spray-dried under the following conditions: Feed rate: 20%, Aspirator: 70%, and 20 atm. The PLGA solution in which the magnetic particles were dispersed was continuously stirred with a stirrer during spray-drying.
6) The spray-dried magnetic particle/PLGA composite powder was thoroughly washed and then dried to completely remove the remaining solvent, and then collected.
<多孔性複合粉体の表面観察>
図2a及び2bを参照すると、表面写真から直径数百ナノメートルの気孔が形成されており、且つ酸化鉄粒子が密に含浸されていることを確認することができた。そして、酸化鉄:PLGA=80:20のサンプルの場合、1gを500℃で180分間処理して高分子を全て燃やしてから減少した重さを測定する方式にて実際の強熱減量(loss on ignition)を測定した結果、19~21%の水準であり、このことから、複合粉体の内部にも酸化鉄が均一に含浸されているということを確認することができた。
<Surface observation of porous composite powder>
2a and 2b, it was confirmed that pores with a diameter of several hundred nanometers were formed and that iron oxide particles were densely impregnated from the surface photographs.In addition, in the case of a sample of iron oxide:PLGA=80:20, the actual loss on ignition was measured by treating 1g at 500°C for 180 minutes to burn off all the polymer and then measuring the weight loss, and the result was 19-21%, which confirmed that iron oxide was uniformly impregnated inside the composite powder.
<多孔性複合粉体の気孔構造の確認>
AP球のポア構造を確認した結果、図10a及び10bを参照すると、浸透体積(Total Intrusion Volume)は0.62mL/gであって、後述する吸油量測定装備(S-500、Asahi Souken社製、図3a及び3b)を用いて測定された吸油量(0.48mL/g)と類似の水準を示すのが確認された。また、平均気孔直径(Average Pore Diameter(4V/A))は0.33μmであって、前記SEMイメージ上のポアの直径(図2a及び2b)と類似した値を示した。
<Confirmation of the pore structure of the porous composite powder>
As a result of examining the pore structure of the AP sphere, referring to Figures 10a and 10b, the total intrusion volume was 0.62 mL/g, which was confirmed to be similar to the oil absorption (0.48 mL/g) measured using an oil absorption measurement device (S-500, manufactured by Asahi Souken, Figures 3a and 3b) described below. In addition, the average pore diameter (4V/A) was 0.33 μm, which was similar to the pore diameter on the SEM image (Figures 2a and 2b).
また、実際に皮脂を吸油することができる気孔の全体割合を意味する孔隙率(Porosity)は、実施例の場合は61%の水準であって、これは酸化鉄粒子を80%も含浸しているにも拘わらず、内部気孔構造を保持していることから奏される効果である。 In addition, the porosity, which means the total percentage of pores that can actually absorb sebum, is at a level of 61% in the example, which is an effect achieved by maintaining the internal pore structure despite being impregnated with 80% iron oxide particles.
実験例 - 吸油量テスト
AP球が細塵を含んでいる皮脂を気孔内部へと有効に吸いこむことができるかどうかを確認するために、保有中の吸油量測定装備(S-500、Asahi Souken社製、図3a及び3b)を用いて、皮脂と最も類似した物性を有するMCTオイル(CAS.No73398-61-5)に対する吸油量を、下記のような方法にてテストし、その結果を図4に示した。
Experimental Example - Oil Absorption Test In order to confirm whether the AP ball can effectively absorb sebum containing fine dust into the pores, the oil absorption test was performed on MCT oil (CAS. No. 73398-61-5) which has the most similar physical properties to sebum, using an oil absorption tester (S-500, manufactured by Asahi Souken, Figures 3a and 3b) in the following manner, and the results are shown in Figure 4.
1)測定対象のパウダーの重さを測定した後、サンプルチャンバ(chamber)に投入した。
2)吸油量測定装備が作動を開始すると、オイルポンプがオイルを一滴ずつチャンバ(chamber)の中に落とし、チャンバ(chamber)中では2台のミキサーが回転をしながらパウダーとオイルとを練りこんだ。
3)投入されるオイルの量が増加するに伴い、ミキサーにかかるトルク(Torque)値も増加していき、最大値に達したところで試験を完了した。
4)このとき、最大トルク(Torque)の70%に該当するオイルの量(ml)を試料の量で除算した値をパウダーの吸油量(ml/g)として算出した。具体的に、オイル量14.09ml、試料量29.35gであって、吸油量の値は14.09/29.35=0.48ml/gと算出された。
1) The powder to be measured was weighed and then placed in a sample chamber.
2) When the oil absorption measuring equipment started to operate, the oil pump dropped oil drop by drop into the chamber, where two mixers rotated to mix the powder and oil.
3) As the amount of oil added increased, the torque applied to the mixer also increased, and the test was completed when it reached a maximum value.
4) The amount of oil (ml) corresponding to 70% of the maximum torque was divided by the amount of sample to calculate the oil absorption (ml/g) of the powder. Specifically, the amount of oil was 14.09 ml, the amount of sample was 29.35 g, and the oil absorption value was calculated as 14.09/29.35=0.48 ml/g.
図4を参照すると、酸化鉄自体の吸油量は0.28ml/gであるが、PLGA内部に酸化鉄を含浸させたAP球の場合は吸油量が0.48ml/gとほぼ2倍程度大きく増加することを確認した。これは、AP球が酸化鉄を80%も含有しているにも拘わらず、複合粉体の表面と内部に多数の気孔が形成されていて孔隙率(porosity)が保持されることで生じる効果である。よって、酸化鉄を単独で用いる場合よりはAP球を用いる場合のほうが皮脂に含まれた細塵をより多量吸いこむことができ、且つ、気孔内部に捕獲することから有害な細塵を肌から隔離させる効果が大きいといえる。 Referring to Figure 4, the oil absorption of iron oxide itself is 0.28 ml/g, but in the case of AP spheres with iron oxide impregnated inside PLGA, the oil absorption is 0.48 ml/g, which is almost double. This is because, even though the AP spheres contain 80% iron oxide, numerous pores are formed on the surface and inside of the composite powder, maintaining porosity. Therefore, it can be said that the use of AP spheres is more effective at absorbing fine dust contained in sebum than the use of iron oxide alone, and is more effective at isolating harmful fine dust from the skin by capturing it inside the pores.
実験例 - 重金属吸入シミュレーション
細塵がAP球の内部に実際に吸いこまれるかどうかを確認するために、5大重金属スタンダードソリューション(Cd、Hg、Sb、Pb、Asのそれぞれを200ppm)をAP球に1時間十分に吸収させてから乾燥し、SEM-EDX Mapping(電子顕微鏡元素分析)によってそれぞれの元素毎に異なる色相にて定性分析した結果を図5に示した。実験の結果、AP球粒子の内部に5大重金属元素が実際に均一に分布していることを確認することができた。
Experimental Example - Heavy Metal Inhalation Simulation To confirm whether fine dust is actually inhaled inside the AP sphere, a standard solution of the five major heavy metals (Cd, Hg, Sb, Pb, As each at 200 ppm) was fully absorbed into the AP sphere for one hour, and then it was dried and qualitatively analyzed by SEM-EDX Mapping (electron microscope elemental analysis) with different hues for each element, the results of which are shown in Figure 5. As a result of the experiment, it was confirmed that the five major heavy metal elements are actually distributed uniformly inside the AP sphere particles.
実験例 - 細塵除去性能評価
毛穴模倣体として、複数の50μm直径の人工毛穴及び複数の200μm直径の人工毛穴を有する毛穴模倣体の製造が可能な金属鋳型(metal mold)を製作した後、前記鋳型にポリジメチルシロキサン(polydimethylsiloxane、PDMS;SYLGARD(登録商標) 184(Sigma社製、アメリカ)を原料として使用)をコートし、前記PDMSが完全に硬化したときに鋳型から取り出して毛穴模倣体を得た。そして、細塵ミミック素材としては、500nm以下のカーボンブラックナノ粒子を用い、下記のようにAP球の細塵除去性能を評価し、図6に示した。
Experimental Example - Evaluation of Fine Dust Removal Performance A metal mold capable of manufacturing a pore mimic having multiple artificial pores with a diameter of 50 μm and multiple artificial pores with a diameter of 200 μm was fabricated, and then the mold was coated with polydimethylsiloxane (PDMS; SYLGARD® 184 (Sigma, USA) was used as a raw material), and when the PDMS was completely cured, it was removed from the mold to obtain a pore mimic. Carbon black nanoparticles of 500 nm or less were used as the fine dust mimic material, and the fine dust removal performance of the AP sphere was evaluated as follows, and the results are shown in Figure 6.
1)MCT(Medium Chain Triglyceride oil)オイルとB.G.(Butylene Glycol)及びカーボンブラックを特定の割合(MCTオイル:B.G.:カーボンブラック=77.9:20.8:1.3)で混合して細塵溶液を製造した。
2)前記1)で製造した細塵溶液とは別に、AP球(PLGA+酸化鉄)とMCTオイルを50:50の割合で混合し、細塵除去用多孔性複合粉体を含む組成物を製造した。
3)毛穴模倣体の表面に細塵溶液を塗った後、その上に細塵除去用多孔性複合粉体を含む組成物を塗布した。
4)ティッシュ及びティッシュで包んだ磁石(1000Gauss)でそれぞれ毛穴模倣体の表面を30回ずつ擦ってから、顕微鏡にてその表面を観察した。
1) A fine dust solution was prepared by mixing MCT (Medium Chain Triglyceride oil), BG (Butylene Glycol) and carbon black in a specific ratio (MCT oil: BG: carbon black = 77.9: 20.8: 1.3).
2) Separately from the fine dust solution prepared in 1), AP spheres (PLGA + iron oxide) and MCT oil were mixed in a ratio of 50:50 to prepare a composition containing porous composite powder for removing fine dust.
3) After the fine dust solution was applied to the surface of the pore mimic, a composition containing a fine dust removing porous composite powder was applied thereon.
4) The surface of the pore mimic was rubbed 30 times each with a tissue and a magnet (1000 Gauss) wrapped in the tissue, and then the surface was observed under a microscope.
図6a及び6bを参照すると、ティッシュだけで除去したときは、毛穴内部のカーボンブラックはほとんど除去されていないのに対し、ティッシュで包んだ磁石で除去したときは、毛穴内部のカーボンブラックが大部分除去されたことを観察することができた。このことから、磁性が与えられた多孔性粒子であるAP球が毛穴模倣体内部のカーボンブラックを吸いこみ、外部から磁力を加えると、簡易に毛穴から脱着が可能であることが確認された。 Referring to Figures 6a and 6b, it was observed that when the carbon black was removed using only tissue, almost none of the carbon black inside the pores was removed, whereas when the carbon black was removed using a magnet wrapped in tissue, most of the carbon black inside the pores was removed. This confirmed that the AP spheres, which are porous particles that have been given magnetism, can absorb the carbon black inside the pore mimics, and when magnetic force is applied from the outside, they can be easily detached from the pores.
実験例 - 磁性の強さ測定
実施例で製造されたAP球の酸化鉄含浸割合を50重量%、80重量%及び100重量%(100%の場合、単に磁性を相対比較するための酸化鉄サンプル)にし、それによる磁性の強さを測定した。図9を参照すると、磁性の強さは、磁性粒子(酸化鉄)の割合に正比例することを確認することができ、実施例で製造されたように酸化鉄を80重量%含浸する場合、磁性の強さも100%の酸化鉄に対して約80%程度に減少したことを確認した。
Experimental Example - Magnetic Strength Measurement The AP spheres manufactured in the examples were impregnated with iron oxide at 50%, 80% and 100% by weight (100% was an iron oxide sample for simply comparing magnetic properties), and the magnetic strength was measured. Referring to Figure 9, it was confirmed that the magnetic strength is directly proportional to the proportion of magnetic particles (iron oxide), and that when 80% by weight of iron oxide was impregnated as in the examples, the magnetic strength was reduced to about 80% compared to 100% iron oxide.
Claims (17)
前記多孔性複合粉体は、
高分子、及び
前記高分子に含浸された磁性粒子を含み、
前記多孔性複合粉体の粒径は、20~100μmの範囲であり、
前記高分子は、生分解性高分子である細塵除去用多孔性複合粉体。 A porous composite powder for removing fine dust, comprising:
The porous composite powder is
a polymer; and magnetic particles impregnated in the polymer;
The particle size of the porous composite powder is in the range of 20 to 100 μm;
The porous composite powder for removing fine dust is a biodegradable polymer .
マグネチックアプリケータを用いて前記多孔性複合粉体を肌から脱着する段階、を含む細塵除去方法。 A method for removing fine dust, comprising: applying the composition according to any one of claims 10 to 12 onto the skin; and detaching the porous composite powder from the skin using a magnetic applicator.
高分子を含む溶液を製造する段階と、
磁性粒子を前記高分子を含む溶液に分散させる段階、及び
前記磁性粒子が分散された溶液を噴霧乾燥する段階と、を含む細塵除去用多孔性複合粉体の製造方法。 A method for producing the porous composite powder according to any one of claims 1 to 9 , comprising the steps of:
Producing a solution comprising a polymer;
A method for producing a porous composite powder for removing fine dust, comprising: dispersing magnetic particles in a solution containing the polymer; and spray-drying the solution in which the magnetic particles are dispersed.
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