WO2023140123A1 - Cosmetic containing zinc oxide particles - Google Patents
Cosmetic containing zinc oxide particles Download PDFInfo
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- WO2023140123A1 WO2023140123A1 PCT/JP2023/000137 JP2023000137W WO2023140123A1 WO 2023140123 A1 WO2023140123 A1 WO 2023140123A1 JP 2023000137 W JP2023000137 W JP 2023000137W WO 2023140123 A1 WO2023140123 A1 WO 2023140123A1
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- Prior art keywords
- zinc oxide
- oxide particles
- cosmetic
- sebum
- surface area
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/27—Zinc; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/12—Face or body powders for grooming, adorning or absorbing
Definitions
- the present invention relates to cosmetics containing zinc oxide particles. More specifically, the present invention relates to a cosmetic composition that contains zinc oxide particles that are spherical and have excellent sebum-solidifying effects, thereby achieving both a high effect of preventing makeup deterioration and a smooth texture when used.
- Sebum has the role of preventing foreign matter from entering from the outside and suppressing evaporation of water from the skin. However, when it is secreted excessively, it may cause cosmetic troubles such as shine, stickiness, makeup failure, conspicuous pores, and acne. Sebum contains many unsaturated fatty acids such as stearic acid, oleic acid, linoleic acid, palmitic acid, sapienic acid, and palmitoleic acid. Therefore, efficient solidification of oleic acid is effective in preventing cosmetic troubles.
- Patent Document 1 discloses a sebum-resistant powder obtained by surface-treating microparticles of zinc oxide having a specific surface area of 15 to 100 m 2 /g with a specific methylhydrogensiloxane/dimethylsiloxane copolymer, and a cosmetic containing the same, which is said to have an excellent sebum control effect and improve makeup longevity.
- Patent Document 2 discloses an unsaturated fatty acid adsorbent composed of plate-shaped accumulated spherical zinc oxide having a median diameter of 0.01 ⁇ m or more and less than 10 ⁇ m and a D90/D10 of 5.0 or less, and a cosmetic containing the same. It is said that the adsorbent not only has a high ultraviolet shielding ability, but also suppresses the spread of the sebum by fixing the sebum, so that the makeup does not easily fall off and the feeling of use is good.
- Patent Document 3 discloses a zinc oxide powder for a makeup cosmetic that is a plate-shaped zinc oxide powder, has pores in the plate-shaped zinc oxide particles that constitute the powder, and has a pore size of 0.05 to 1 ⁇ m, and a makeup cosmetic containing the zinc oxide powder.
- the zinc oxide blended in these cosmetics may not have a sufficient sebum-solidifying effect, and when blended in the cosmetics, it may cause a squeaky feeling when applied, and the feeling of use may be inferior.
- JP-A-8-41379 JP 2018-083765 A Japanese Patent Application Laid-Open No. 2020-019720
- the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a cosmetic that contains zinc oxide particles, has a sufficient sebum-solidifying effect, and also has an excellent feel when used.
- the inventors found that the sebum-solidifying effect and improvement of feel during use can be achieved at the same time by blending zinc oxide particles that satisfy predetermined shapes and physical properties, and have completed the present invention.
- the gist of the present invention is a cosmetic containing spherical zinc oxide particles having a median diameter (D50) of 1 to 300 ⁇ m and a BET specific surface area of 20 m 2 /g or more.
- zinc oxide particles having a BET specific surface area of 110 to 130 m 2 /g are preferred.
- the zinc oxide particles preferably have a pore diameter peak of 7 nm or more.
- the zinc oxide particles blended in the cosmetic of the present invention exhibit a particularly excellent effect in solidifying oleic acid by having a predetermined specific surface area. For this reason, the cosmetic of the present invention exhibits the action and effect of preventing the occurrence of shine and makeup deterioration due to sebum and making the makeup last longer. Furthermore, since the zinc oxide particles blended in the cosmetic of the present invention have a predetermined shape and particle size, compared to cosmetics containing conventional zinc oxide particles having a plate-like shape, a columnar shape, or a shape in which these are accumulated, or conventional zinc oxide particles having a nano-sized particle size, it is possible to realize a smooth feeling in use without a squeaky feeling.
- the cosmetic of the present invention essentially contains zinc oxide particles having a predetermined shape and physical properties. A detailed description will be given below.
- the zinc oxide particles that can be used in the present invention have spherical and porous primary particles, and are characterized by the shape, particle size and specific surface area of the primary particles.
- the zinc oxide particles that can be used in the present invention have a spherical primary particle shape.
- the term "spherical” does not mean only true spheres, but may also be elliptical, approximately spherical, or have fine holes or irregularities on the surface. In the case of an elliptical shape or a substantially spherical shape, it is preferable that the ratio of the minor axis to the major axis is 1:1 to 1:2. Since the zinc oxide particles have a spherical shape, they can be applied smoothly and impart a smooth feel.
- the zinc oxide particles that can be used in the present invention have a median diameter (D50) of primary particles in the range of 1 to 300 ⁇ m.
- the median diameter (D50) refers to the particle diameter ( ⁇ m) when the cumulative volume obtained by accumulating the particle diameters of the zinc oxide particles from the smaller particle diameter side is 50%.
- Particle size can be measured with a laser diffraction particle size distribution analyzer.
- the lower limit of the median diameter (D50) is 1 ⁇ m or more, more preferably 2 ⁇ m or more, still more preferably 3 ⁇ m or more, and particularly preferably 5 ⁇ m or more.
- the upper limit is 300 ⁇ m or less, more preferably 100 ⁇ m or less, still more preferably 50 ⁇ m or less, and particularly preferably 15 ⁇ m or less.
- the zinc oxide particles that can be used in the present invention have a BET specific surface area of 20 m 2 /g or more.
- the BET specific surface area can be measured using a fully automatic specific surface area meter.
- the lower limit of the BET specific surface area is 20 m 2 /g or more, more preferably 70 m 2 /g or more, still more preferably 100 m 2 /g or more, and particularly preferably 110 m 2 /g or more.
- the upper limit of the BET specific surface area is not particularly limited, because the sebum-solidifying effect generally tends to improve as the value of the BET specific surface area increases.
- the range of the BET specific surface area of zinc oxide particles is, for example, 110 to 130 m 2 /g.
- the efficiency of sebum solidification can be increased.
- zinc oxide particles having a BET specific surface area of 110 m 2 /g or more are particularly preferable because they can exert a sebum-solidifying effect immediately after being applied to the skin.
- the cosmetic composition of the present invention containing zinc oxide particles satisfying these conditions as a sebum solidifying agent is excellent in terms of longevity and feel during use.
- the pore diameter on the surface of the zinc oxide particles further satisfies the following condition (4).
- the lower limit of the pore diameter peak of zinc oxide particles is preferably 7 nm or more, more preferably 8 nm or more, and particularly preferably 10 nm or more.
- the pore diameter peak generally tends to improve the sebum-solidifying effect as the value increases, so the upper limit is not particularly limited, but in consideration of availability and other physical properties, it can be, for example, 100 nm or less, 80 nm or less, or 50 nm or less.
- the "pore size peak” is the peak of the pore size distribution calculated by the BJH (Barrett Joyner Hallenda) method.
- the zinc oxide particles having the above-described shape and physical properties can be produced by heating an aqueous solution containing a zinc compound and ammonium ions to obtain a precipitate of basic zinc carbonate, and then firing, pulverizing, and spray-drying the obtained basic zinc carbonate.
- the particle shape, particle size, specific surface area and pore size can be adjusted by appropriately changing the pulverization, spraying conditions and firing conditions.
- the content of zinc oxide particles in the cosmetic of the present invention is not particularly limited, but the lower limit is preferably 1.0% by mass or more, more preferably 5.0% by mass or more, and particularly preferably 10.0% by mass or more.
- the upper limit is preferably 50.0% by mass or less, more preferably 30% by mass or less, and particularly preferably 20.0% by mass or less. Therefore, the content range of the zinc oxide particles is, for example, 10.0 to 20.0% by mass.
- the cosmetic of the present invention is not particularly limited, and includes general cosmetics such as skin care cosmetics such as face wash cream, lotion, massage cream, milky lotion, and moisture cream; makeup cosmetics such as foundation, face powder, makeup base, face powder, eye shadow, eyeliner, lipstick, and blush; body care cosmetics such as bath salts, sunscreen creams, and deodorant sprays; Excellent effects can be exhibited by being blended into makeup bases, face powders, makeup bases, and face powders.
- skin care cosmetics such as face wash cream, lotion, massage cream, milky lotion, and moisture cream
- makeup cosmetics such as foundation, face powder, makeup base, face powder, eye shadow, eyeliner, lipstick, and blush
- body care cosmetics such as bath salts, sunscreen creams, and deodorant sprays
- Excellent effects can be exhibited by being blended into makeup bases, face powders, makeup bases, and face powders.
- the cosmetic composition of the present invention can contain other ingredients that are commonly used in cosmetics, depending on the application.
- Main examples include powders, oils, and aqueous components.
- water-soluble polymer compounds, thickeners, ultraviolet absorbers, sequestering agents, amino acids, skin nutrients, blood circulation promoters, antiperspirants, bactericides, antiphlogistic agents, antioxidants, preservatives, fragrances, and the like can be added.
- the powder that can be blended in the cosmetic of the present invention is not particularly limited, but for example, talc, sericite, mica, kaolin, magnesium carbonate, calcium carbonate, aluminum silicate, barium silicate, calcium silicate, magnesium silicate, strontium silicate, metal tungstate, magnesium, silica, zeolite, barium sulfate, calcined calcium sulfate, calcium phosphate, fluoroapatite, hydroxyapatite, metallic soap, boron nitride, nylon powder, polyethylene powder, cellulose powder, silicone powder, zinc oxide.
- Extender pigments such as carbon black, titanium oxide, ultramarine blue, Prussian blue, chromium oxide, organic tar pigments, lakes, and other coloring agents; mica titanium, iron oxide-coated mica and other composite pigments; silicone compounds, fluorine-modified silicone compounds, fluorine compounds, higher fatty acids, higher alcohols, fatty acid esters, metal soaps, amino acids, quaternary ammonium salts, alkyl phosphates, and the like.
- the oil that can be blended in the cosmetic of the present invention is not particularly limited as long as it can be used in general cosmetics, and includes hydrocarbon oil, synthetic ester oil, silicone oil, and the like. From the viewpoints of usability, feeling of use, etc., it is preferable that silicone oil is included.
- Aqueous components that can be blended in the cosmetics of the present invention can be used without any particular restrictions as long as they are water-soluble components.
- aqueous components include lower alcohols such as ethyl alcohol, chelating agents, pH adjusters, preservatives, and the like.
- the present invention will be described in more detail below with reference to examples, but the present invention is not limited by these.
- the blending amount is shown in % by mass relative to the system in which the component is blended.
- the BET specific surface area was measured using BELSORP-miniII manufactured by Microtrack Bell Co., Ltd.
- ⁇ Pore size peak> For each sample of zinc oxide particles, the amount of nitrogen gas adsorbed at each pressure was determined using a gas adsorption type pore distribution measuring device, and the cumulative pore volume distribution and pore distribution calculated by the BJH method were obtained. A pore size peak was determined from the distribution.
- a powder cosmetic (foundation) having the following composition was prepared for each sample of zinc oxide particles. Specifically, the following components were mixed in a Henschel mixer, pulverized in a pulperizer, filled in a resin-made medium dish container, and dry-pressed by a known method to obtain a powdered cosmetic.
- Foundation (ingredient name) Amount (% by mass) Talc Balance zinc oxide particles (any of samples 1 to 18) 5 mica 20 Titanium oxide 10 Dimethicone 25 Methylphenylpolysiloxane 5
- the resulting powdery cosmetic was evaluated for feel in use (smoothness, absence of squeaky feeling) when applied to the skin by the following methods.
- a panel of 20 cosmetics evaluation specialists used the powdered cosmetics, evaluated the feeling of use in five stages according to the following criteria, assigned a score to each cosmetic, and further evaluated the average score of all the panels according to the following four-stage judgment criteria.
- the spherical zinc oxide particles having a median diameter (D50) of 1 to 300 ⁇ m, a BET specific surface area of 20 m 2 /g or more, and having a sufficient sebum-solidifying effect exhibited an excellent feel during use when blended in cosmetics (Samples 1 to 10).
- D50 median diameter
- BET specific surface area 20 m 2 /g or more
- sebum-solidifying effect immediately after being shaken
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Abstract
The purpose of this invention is to provide a cosmetic that contains zinc oxide particles and that has a sufficient sebum-solidifying effect while also having an excellent texture when used. The cosmetic according to the present invention is characterized by containing spherical zinc oxide particles having a median diameter (D50) of 1 to 300 μm and a BET specific surface area of 20 m2/g or greater.
Description
本発明は、酸化亜鉛粒子を含有する化粧料に関する。より詳しくは、球状かつ皮脂固化効果に優れた酸化亜鉛粒子を含有することにより、高い化粧崩れ防止効果と滑らかな使用感触とを両立した化粧料に関する。
The present invention relates to cosmetics containing zinc oxide particles. More specifically, the present invention relates to a cosmetic composition that contains zinc oxide particles that are spherical and have excellent sebum-solidifying effects, thereby achieving both a high effect of preventing makeup deterioration and a smooth texture when used.
皮脂は外界から異物が侵入するのを防ぎ、肌からの水分蒸散を抑制する役割を有する。しかし、過剰に分泌されると、美容上のトラブル、例えば、テカリ、べたつき、化粧崩れ、毛穴の目立ち、にきびの発生などを引き起こす場合がある。
皮脂には、ステアリン酸、オレイン酸、リノール酸、パルミチン酸、サピエン酸、パルミトレイン酸等の多くの不飽和脂肪酸が含まれており、これらの中でも、オレイン酸は皮脂の代表的な成分であり、一定の比率を占める。このため、オレイン酸を効率良く固化することが美容上のトラブルを防止する上で有効である。 Sebum has the role of preventing foreign matter from entering from the outside and suppressing evaporation of water from the skin. However, when it is secreted excessively, it may cause cosmetic troubles such as shine, stickiness, makeup failure, conspicuous pores, and acne.
Sebum contains many unsaturated fatty acids such as stearic acid, oleic acid, linoleic acid, palmitic acid, sapienic acid, and palmitoleic acid. Therefore, efficient solidification of oleic acid is effective in preventing cosmetic troubles.
皮脂には、ステアリン酸、オレイン酸、リノール酸、パルミチン酸、サピエン酸、パルミトレイン酸等の多くの不飽和脂肪酸が含まれており、これらの中でも、オレイン酸は皮脂の代表的な成分であり、一定の比率を占める。このため、オレイン酸を効率良く固化することが美容上のトラブルを防止する上で有効である。 Sebum has the role of preventing foreign matter from entering from the outside and suppressing evaporation of water from the skin. However, when it is secreted excessively, it may cause cosmetic troubles such as shine, stickiness, makeup failure, conspicuous pores, and acne.
Sebum contains many unsaturated fatty acids such as stearic acid, oleic acid, linoleic acid, palmitic acid, sapienic acid, and palmitoleic acid. Therefore, efficient solidification of oleic acid is effective in preventing cosmetic troubles.
酸化亜鉛は皮脂に含まれる脂肪酸を金属石鹸化して固化させる作用を有することが知られており、これまでにも皮脂の固化を目的として酸化亜鉛を配合した種々の化粧料が提案されている。
例えば、特許文献１には、比表面積が１５～１００ｍ２／ｇである微粒子酸化亜鉛を特定のメチルハイドロジェンシロキサン・ジメチルシロキサン共重合体で表面処理した耐皮脂粉体とそれを含有する化粧料が開示されており、皮脂コントロール効果に優れ、化粧持ちを向上させることができるとされている。 Zinc oxide is known to have the effect of turning fatty acids contained in sebum into metallic soap and solidifying them, and various cosmetics containing zinc oxide have been proposed for the purpose of solidifying sebum.
For example, Patent Document 1 discloses a sebum-resistant powder obtained by surface-treating microparticles of zinc oxide having a specific surface area of 15 to 100 m 2 /g with a specific methylhydrogensiloxane/dimethylsiloxane copolymer, and a cosmetic containing the same, which is said to have an excellent sebum control effect and improve makeup longevity.
例えば、特許文献１には、比表面積が１５～１００ｍ２／ｇである微粒子酸化亜鉛を特定のメチルハイドロジェンシロキサン・ジメチルシロキサン共重合体で表面処理した耐皮脂粉体とそれを含有する化粧料が開示されており、皮脂コントロール効果に優れ、化粧持ちを向上させることができるとされている。 Zinc oxide is known to have the effect of turning fatty acids contained in sebum into metallic soap and solidifying them, and various cosmetics containing zinc oxide have been proposed for the purpose of solidifying sebum.
For example, Patent Document 1 discloses a sebum-resistant powder obtained by surface-treating microparticles of zinc oxide having a specific surface area of 15 to 100 m 2 /g with a specific methylhydrogensiloxane/dimethylsiloxane copolymer, and a cosmetic containing the same, which is said to have an excellent sebum control effect and improve makeup longevity.
また、特許文献２には、メジアン径０．０１μｍ以上１０μｍ未満であり、Ｄ９０／Ｄ１０が５．０以下である板状集積型球状酸化亜鉛からなる不飽和脂肪酸吸着剤とそれを含む化粧料が開示されており、高い紫外線遮蔽能を有するだけでなく、皮脂を固定化して皮脂の広がりを抑制することにより、化粧崩れを起こしにくく、使用感も良好であるとされている。
さらに、特許文献３には、板状の酸化亜鉛粉末であって、粉末を構成する板状酸化亜鉛の粒子に細孔を有し、細孔の孔径が０．０５～１μｍであるメイクアップ化粧料用の酸化亜鉛粉末とそれを含むメイクアップ化粧料が開示されており、化粧崩れが発生しにくく、化粧持ちが良いとされている。 In addition, Patent Document 2 discloses an unsaturated fatty acid adsorbent composed of plate-shaped accumulated spherical zinc oxide having a median diameter of 0.01 μm or more and less than 10 μm and a D90/D10 of 5.0 or less, and a cosmetic containing the same. It is said that the adsorbent not only has a high ultraviolet shielding ability, but also suppresses the spread of the sebum by fixing the sebum, so that the makeup does not easily fall off and the feeling of use is good.
Furthermore, Patent Document 3 discloses a zinc oxide powder for a makeup cosmetic that is a plate-shaped zinc oxide powder, has pores in the plate-shaped zinc oxide particles that constitute the powder, and has a pore size of 0.05 to 1 μm, and a makeup cosmetic containing the zinc oxide powder.
さらに、特許文献３には、板状の酸化亜鉛粉末であって、粉末を構成する板状酸化亜鉛の粒子に細孔を有し、細孔の孔径が０．０５～１μｍであるメイクアップ化粧料用の酸化亜鉛粉末とそれを含むメイクアップ化粧料が開示されており、化粧崩れが発生しにくく、化粧持ちが良いとされている。 In addition, Patent Document 2 discloses an unsaturated fatty acid adsorbent composed of plate-shaped accumulated spherical zinc oxide having a median diameter of 0.01 μm or more and less than 10 μm and a D90/D10 of 5.0 or less, and a cosmetic containing the same. It is said that the adsorbent not only has a high ultraviolet shielding ability, but also suppresses the spread of the sebum by fixing the sebum, so that the makeup does not easily fall off and the feeling of use is good.
Furthermore, Patent Document 3 discloses a zinc oxide powder for a makeup cosmetic that is a plate-shaped zinc oxide powder, has pores in the plate-shaped zinc oxide particles that constitute the powder, and has a pore size of 0.05 to 1 μm, and a makeup cosmetic containing the zinc oxide powder.
しかし、これらの化粧料に配合されている酸化亜鉛は、皮脂固化効果が十分でない場合や、化粧料に配合すると塗布の際にきしみ感を生じることがあり、使用感触に劣る場合があった。
However, the zinc oxide blended in these cosmetics may not have a sufficient sebum-solidifying effect, and when blended in the cosmetics, it may cause a squeaky feeling when applied, and the feeling of use may be inferior.
本発明は、前記実情に鑑みてなされたものであり、酸化亜鉛粒子を含有し、十分な皮脂固化効果を有しながら、使用感触にも優れた化粧料を提供することを目的とする。
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a cosmetic that contains zinc oxide particles, has a sufficient sebum-solidifying effect, and also has an excellent feel when used.
本発明者らは上記の課題を解決すべく鋭意研究を行った結果、所定の形状及び物性を満たす酸化亜鉛粒子を配合することにより、皮脂固化効果及び使用感触の改善を同時に実現できることを見出し、本発明を完成するに至った。
As a result of intensive research to solve the above problems, the inventors found that the sebum-solidifying effect and improvement of feel during use can be achieved at the same time by blending zinc oxide particles that satisfy predetermined shapes and physical properties, and have completed the present invention.
すなわち、本発明は、メディアン径（Ｄ５０）が１～３００μｍであり、かつ、ＢＥＴ比表面積が２０ｍ２／ｇ以上である、球状の酸化亜鉛粒子を含有する化粧料を要旨とするものである。
That is, the gist of the present invention is a cosmetic containing spherical zinc oxide particles having a median diameter (D50) of 1 to 300 μm and a BET specific surface area of 20 m 2 /g or more.
特に、酸化亜鉛粒子のＢＥＴ比表面積が１１０～１３０ｍ２／ｇであるものが好ましい。
また、酸化亜鉛粒子は、細孔径のピークが７ｎｍ以上であることが好ましい。 In particular, zinc oxide particles having a BET specific surface area of 110 to 130 m 2 /g are preferred.
Moreover, the zinc oxide particles preferably have a pore diameter peak of 7 nm or more.
また、酸化亜鉛粒子は、細孔径のピークが７ｎｍ以上であることが好ましい。 In particular, zinc oxide particles having a BET specific surface area of 110 to 130 m 2 /g are preferred.
Moreover, the zinc oxide particles preferably have a pore diameter peak of 7 nm or more.
本発明の化粧料に配合される酸化亜鉛粒子は、所定の比表面積を有することにより、オレイン酸の固化に特に優れた効果を発揮する。このため、本発明の化粧料は、皮脂によるテカリや化粧崩れの発生を防ぎ、化粧持ちが良いという作用効果を発揮する。
さらに、本発明の化粧料に配合される酸化亜鉛粒子は、所定の形状及び粒径を有するため、板状、柱状、あるいはこれらが集積した形状等の従来の酸化亜鉛粒子やナノサイズの粒子径を有する従来の酸化亜鉛粒子を含む化粧料と比べて、きしみ感のない滑らかな使用感触を実現することができる。 The zinc oxide particles blended in the cosmetic of the present invention exhibit a particularly excellent effect in solidifying oleic acid by having a predetermined specific surface area. For this reason, the cosmetic of the present invention exhibits the action and effect of preventing the occurrence of shine and makeup deterioration due to sebum and making the makeup last longer.
Furthermore, since the zinc oxide particles blended in the cosmetic of the present invention have a predetermined shape and particle size, compared to cosmetics containing conventional zinc oxide particles having a plate-like shape, a columnar shape, or a shape in which these are accumulated, or conventional zinc oxide particles having a nano-sized particle size, it is possible to realize a smooth feeling in use without a squeaky feeling.
さらに、本発明の化粧料に配合される酸化亜鉛粒子は、所定の形状及び粒径を有するため、板状、柱状、あるいはこれらが集積した形状等の従来の酸化亜鉛粒子やナノサイズの粒子径を有する従来の酸化亜鉛粒子を含む化粧料と比べて、きしみ感のない滑らかな使用感触を実現することができる。 The zinc oxide particles blended in the cosmetic of the present invention exhibit a particularly excellent effect in solidifying oleic acid by having a predetermined specific surface area. For this reason, the cosmetic of the present invention exhibits the action and effect of preventing the occurrence of shine and makeup deterioration due to sebum and making the makeup last longer.
Furthermore, since the zinc oxide particles blended in the cosmetic of the present invention have a predetermined shape and particle size, compared to cosmetics containing conventional zinc oxide particles having a plate-like shape, a columnar shape, or a shape in which these are accumulated, or conventional zinc oxide particles having a nano-sized particle size, it is possible to realize a smooth feeling in use without a squeaky feeling.
本発明の化粧料は、所定の形状及び物性を有する酸化亜鉛粒子を必須に含む。以下、詳しく説明する。
The cosmetic of the present invention essentially contains zinc oxide particles having a predetermined shape and physical properties. A detailed description will be given below.
＜酸化亜鉛粒子＞
本発明で使用できる酸化亜鉛粒子は、一次粒子が球状かつ多孔質であり、その一次粒子の形状、粒径、比表面積に特徴を有する。 <Zinc oxide particles>
The zinc oxide particles that can be used in the present invention have spherical and porous primary particles, and are characterized by the shape, particle size and specific surface area of the primary particles.
本発明で使用できる酸化亜鉛粒子は、一次粒子が球状かつ多孔質であり、その一次粒子の形状、粒径、比表面積に特徴を有する。 <Zinc oxide particles>
The zinc oxide particles that can be used in the present invention have spherical and porous primary particles, and are characterized by the shape, particle size and specific surface area of the primary particles.
（１）形状
本発明で使用できる酸化亜鉛粒子は、一次粒子の形状が球状である。本発明において「球状」とは、真球状のみを意味するものではなく、楕円や略球状、表面に微細な穴や凹凸があるものでもよい。楕円状、略球状の場合は短径と長径の比率が１：１～１：２であれば好ましい。酸化亜鉛粒子の形状が球状であることにより、塗布した際に滑りがよく、さらさらとした感触を付与することができる。 (1) Shape The zinc oxide particles that can be used in the present invention have a spherical primary particle shape. In the present invention, the term "spherical" does not mean only true spheres, but may also be elliptical, approximately spherical, or have fine holes or irregularities on the surface. In the case of an elliptical shape or a substantially spherical shape, it is preferable that the ratio of the minor axis to the major axis is 1:1 to 1:2. Since the zinc oxide particles have a spherical shape, they can be applied smoothly and impart a smooth feel.
本発明で使用できる酸化亜鉛粒子は、一次粒子の形状が球状である。本発明において「球状」とは、真球状のみを意味するものではなく、楕円や略球状、表面に微細な穴や凹凸があるものでもよい。楕円状、略球状の場合は短径と長径の比率が１：１～１：２であれば好ましい。酸化亜鉛粒子の形状が球状であることにより、塗布した際に滑りがよく、さらさらとした感触を付与することができる。 (1) Shape The zinc oxide particles that can be used in the present invention have a spherical primary particle shape. In the present invention, the term "spherical" does not mean only true spheres, but may also be elliptical, approximately spherical, or have fine holes or irregularities on the surface. In the case of an elliptical shape or a substantially spherical shape, it is preferable that the ratio of the minor axis to the major axis is 1:1 to 1:2. Since the zinc oxide particles have a spherical shape, they can be applied smoothly and impart a smooth feel.
（２）メディアン径（Ｄ５０）
本発明で使用できる酸化亜鉛粒子は、一次粒子のメディアン径（Ｄ５０）が１～３００μｍの範囲である。
メディアン径（Ｄ５０）とは、酸化亜鉛粒子の粒径を、小粒径側から積算した累計体積が５０％となるときの粒径（μｍ）をいう。粒径の測定は、レーザー回折粒度分布計によって測定することができる。
メディアン径（Ｄ５０）の下限としては、１μｍ以上、より好ましくは２μｍ以上、さらに好ましくは３μｍ以上、特に好ましくは５μｍ以上である。上限としては、３００μｍ以下、より好ましくは１００μｍ以下、さらに好ましくは５０μｍ以下、特に好ましくは１５μｍ以下である。
酸化亜鉛粒子のメディアン径（Ｄ５０）を上記範囲とすることで、化粧料の使用感触を改善することができる。 (2) Median diameter (D50)
The zinc oxide particles that can be used in the present invention have a median diameter (D50) of primary particles in the range of 1 to 300 μm.
The median diameter (D50) refers to the particle diameter (μm) when the cumulative volume obtained by accumulating the particle diameters of the zinc oxide particles from the smaller particle diameter side is 50%. Particle size can be measured with a laser diffraction particle size distribution analyzer.
The lower limit of the median diameter (D50) is 1 µm or more, more preferably 2 µm or more, still more preferably 3 µm or more, and particularly preferably 5 µm or more. The upper limit is 300 µm or less, more preferably 100 µm or less, still more preferably 50 µm or less, and particularly preferably 15 µm or less.
By setting the median diameter (D50) of the zinc oxide particles within the above range, the feeling of use of the cosmetic can be improved.
本発明で使用できる酸化亜鉛粒子は、一次粒子のメディアン径（Ｄ５０）が１～３００μｍの範囲である。
メディアン径（Ｄ５０）とは、酸化亜鉛粒子の粒径を、小粒径側から積算した累計体積が５０％となるときの粒径（μｍ）をいう。粒径の測定は、レーザー回折粒度分布計によって測定することができる。
メディアン径（Ｄ５０）の下限としては、１μｍ以上、より好ましくは２μｍ以上、さらに好ましくは３μｍ以上、特に好ましくは５μｍ以上である。上限としては、３００μｍ以下、より好ましくは１００μｍ以下、さらに好ましくは５０μｍ以下、特に好ましくは１５μｍ以下である。
酸化亜鉛粒子のメディアン径（Ｄ５０）を上記範囲とすることで、化粧料の使用感触を改善することができる。 (2) Median diameter (D50)
The zinc oxide particles that can be used in the present invention have a median diameter (D50) of primary particles in the range of 1 to 300 μm.
The median diameter (D50) refers to the particle diameter (μm) when the cumulative volume obtained by accumulating the particle diameters of the zinc oxide particles from the smaller particle diameter side is 50%. Particle size can be measured with a laser diffraction particle size distribution analyzer.
The lower limit of the median diameter (D50) is 1 µm or more, more preferably 2 µm or more, still more preferably 3 µm or more, and particularly preferably 5 µm or more. The upper limit is 300 µm or less, more preferably 100 µm or less, still more preferably 50 µm or less, and particularly preferably 15 µm or less.
By setting the median diameter (D50) of the zinc oxide particles within the above range, the feeling of use of the cosmetic can be improved.
（３）ＢＥＴ比表面積
本発明で使用できる酸化亜鉛粒子は、ＢＥＴ比表面積が２０ｍ２／ｇ以上である。ＢＥＴ比表面積の測定は、全自動比表面積計によって測定することができる。
ＢＥＴ比表面積の下限としては、２０ｍ２／ｇ以上、より好ましくは７０ｍ２／ｇ以上、さらに好ましくは１００ｍ２／ｇ以上、特に好ましくは１１０ｍ２／ｇ以上である。一方、ＢＥＴ比表面積は、一般にその値が大きいほど皮脂固化効果が向上する傾向があるため、ＢＥＴ比表面積の上限は特に限定されるものではない。入手容易性や他の物性との兼ね合いから、例えば３００ｍ２／ｇ以下、２５０ｍ２／ｇ以下、２００ｍ２／ｇ以下、あるいは１３０ｍ２／ｇ以下とするのが好ましい。よって、酸化亜鉛粒子のＢＥＴ比表面積の範囲としては、例えば１１０～１３０ｍ２／ｇ等が挙げられる。
酸化亜鉛粒子のＢＥＴ比表面積を上記範囲とすることで、皮脂の固化の効率を上げることができる。なかでも、ＢＥＴ比表面積が１１０ｍ２／ｇ以上である酸化亜鉛粒子は、皮膚に塗布した直後から皮脂固化効果を発揮できるため特に好ましい。 (3) BET specific surface area The zinc oxide particles that can be used in the present invention have a BET specific surface area of 20 m 2 /g or more. The BET specific surface area can be measured using a fully automatic specific surface area meter.
The lower limit of the BET specific surface area is 20 m 2 /g or more, more preferably 70 m 2 /g or more, still more preferably 100 m 2 /g or more, and particularly preferably 110 m 2 /g or more. On the other hand, the upper limit of the BET specific surface area is not particularly limited, because the sebum-solidifying effect generally tends to improve as the value of the BET specific surface area increases. It is preferably 300 m 2 /g or less, 250 m 2 /g or less, 200 m 2 /g or less, or 130 m 2 /g or less in consideration of availability and other physical properties. Therefore, the range of the BET specific surface area of zinc oxide particles is, for example, 110 to 130 m 2 /g.
By setting the BET specific surface area of the zinc oxide particles within the above range, the efficiency of sebum solidification can be increased. Among them, zinc oxide particles having a BET specific surface area of 110 m 2 /g or more are particularly preferable because they can exert a sebum-solidifying effect immediately after being applied to the skin.
本発明で使用できる酸化亜鉛粒子は、ＢＥＴ比表面積が２０ｍ２／ｇ以上である。ＢＥＴ比表面積の測定は、全自動比表面積計によって測定することができる。
ＢＥＴ比表面積の下限としては、２０ｍ２／ｇ以上、より好ましくは７０ｍ２／ｇ以上、さらに好ましくは１００ｍ２／ｇ以上、特に好ましくは１１０ｍ２／ｇ以上である。一方、ＢＥＴ比表面積は、一般にその値が大きいほど皮脂固化効果が向上する傾向があるため、ＢＥＴ比表面積の上限は特に限定されるものではない。入手容易性や他の物性との兼ね合いから、例えば３００ｍ２／ｇ以下、２５０ｍ２／ｇ以下、２００ｍ２／ｇ以下、あるいは１３０ｍ２／ｇ以下とするのが好ましい。よって、酸化亜鉛粒子のＢＥＴ比表面積の範囲としては、例えば１１０～１３０ｍ２／ｇ等が挙げられる。
酸化亜鉛粒子のＢＥＴ比表面積を上記範囲とすることで、皮脂の固化の効率を上げることができる。なかでも、ＢＥＴ比表面積が１１０ｍ２／ｇ以上である酸化亜鉛粒子は、皮膚に塗布した直後から皮脂固化効果を発揮できるため特に好ましい。 (3) BET specific surface area The zinc oxide particles that can be used in the present invention have a BET specific surface area of 20 m 2 /g or more. The BET specific surface area can be measured using a fully automatic specific surface area meter.
The lower limit of the BET specific surface area is 20 m 2 /g or more, more preferably 70 m 2 /g or more, still more preferably 100 m 2 /g or more, and particularly preferably 110 m 2 /g or more. On the other hand, the upper limit of the BET specific surface area is not particularly limited, because the sebum-solidifying effect generally tends to improve as the value of the BET specific surface area increases. It is preferably 300 m 2 /g or less, 250 m 2 /g or less, 200 m 2 /g or less, or 130 m 2 /g or less in consideration of availability and other physical properties. Therefore, the range of the BET specific surface area of zinc oxide particles is, for example, 110 to 130 m 2 /g.
By setting the BET specific surface area of the zinc oxide particles within the above range, the efficiency of sebum solidification can be increased. Among them, zinc oxide particles having a BET specific surface area of 110 m 2 /g or more are particularly preferable because they can exert a sebum-solidifying effect immediately after being applied to the skin.
上記の（１）～（３）の条件を満たすことにより、酸化亜鉛粒子は、皮脂を十分に固化しつつ、さらさらとした滑らかな感触を付与する。このため、これらの条件を満たす酸化亜鉛粒子を皮脂固化剤として配合した本願発明の化粧料は、化粧持ちと使用感触の両面に優れている。
なお、より即効性に優れた皮脂固化効果を得るには、上記した（１）～（３）の他に、酸化亜鉛粒子の表面の細孔径が下記（４）の条件をさらに満たすことが好ましい。 By satisfying the above conditions (1) to (3), the zinc oxide particles sufficiently solidify sebum and impart a dry and smooth touch. Therefore, the cosmetic composition of the present invention containing zinc oxide particles satisfying these conditions as a sebum solidifying agent is excellent in terms of longevity and feel during use.
In order to obtain a more immediate sebum-solidifying effect, in addition to the above (1) to (3), it is preferable that the pore diameter on the surface of the zinc oxide particles further satisfies the following condition (4).
なお、より即効性に優れた皮脂固化効果を得るには、上記した（１）～（３）の他に、酸化亜鉛粒子の表面の細孔径が下記（４）の条件をさらに満たすことが好ましい。 By satisfying the above conditions (1) to (3), the zinc oxide particles sufficiently solidify sebum and impart a dry and smooth touch. Therefore, the cosmetic composition of the present invention containing zinc oxide particles satisfying these conditions as a sebum solidifying agent is excellent in terms of longevity and feel during use.
In order to obtain a more immediate sebum-solidifying effect, in addition to the above (1) to (3), it is preferable that the pore diameter on the surface of the zinc oxide particles further satisfies the following condition (4).
（４）細孔径ピーク
酸化亜鉛粒子の細孔径ピークの下限としては、好ましくは７ｎｍ以上、より好ましくは８ｎｍ以上、特に好ましくは１０ｎｍ以上である。酸化亜鉛粒子の細孔径ピークを上記範囲とすることで、皮脂の固化の効率をさらに向上させることができる。一方、細孔径ピークは、一般にその値が大きいほど皮脂固化効果が向上する傾向があるため、上限は特に限定されるものではないが、入手容易性や他の物性との兼ね合いから、例えば１００ｎｍ以下、８０ｎｍ以下、５０ｎｍ以下とすることができる。なお、本発明において「細孔径ピーク」とは、ＢＪＨ（Barrett Joyner Hallenda）法で計算された細孔分布のピークである。 (4) Pore Diameter Peak The lower limit of the pore diameter peak of zinc oxide particles is preferably 7 nm or more, more preferably 8 nm or more, and particularly preferably 10 nm or more. By setting the pore diameter peak of the zinc oxide particles within the above range, the sebum solidification efficiency can be further improved. On the other hand, the pore diameter peak generally tends to improve the sebum-solidifying effect as the value increases, so the upper limit is not particularly limited, but in consideration of availability and other physical properties, it can be, for example, 100 nm or less, 80 nm or less, or 50 nm or less. In the present invention, the "pore size peak" is the peak of the pore size distribution calculated by the BJH (Barrett Joyner Hallenda) method.
酸化亜鉛粒子の細孔径ピークの下限としては、好ましくは７ｎｍ以上、より好ましくは８ｎｍ以上、特に好ましくは１０ｎｍ以上である。酸化亜鉛粒子の細孔径ピークを上記範囲とすることで、皮脂の固化の効率をさらに向上させることができる。一方、細孔径ピークは、一般にその値が大きいほど皮脂固化効果が向上する傾向があるため、上限は特に限定されるものではないが、入手容易性や他の物性との兼ね合いから、例えば１００ｎｍ以下、８０ｎｍ以下、５０ｎｍ以下とすることができる。なお、本発明において「細孔径ピーク」とは、ＢＪＨ（Barrett Joyner Hallenda）法で計算された細孔分布のピークである。 (4) Pore Diameter Peak The lower limit of the pore diameter peak of zinc oxide particles is preferably 7 nm or more, more preferably 8 nm or more, and particularly preferably 10 nm or more. By setting the pore diameter peak of the zinc oxide particles within the above range, the sebum solidification efficiency can be further improved. On the other hand, the pore diameter peak generally tends to improve the sebum-solidifying effect as the value increases, so the upper limit is not particularly limited, but in consideration of availability and other physical properties, it can be, for example, 100 nm or less, 80 nm or less, or 50 nm or less. In the present invention, the "pore size peak" is the peak of the pore size distribution calculated by the BJH (Barrett Joyner Hallenda) method.
＜酸化亜鉛粒子の製法＞
上記の形状及び物性を有する酸化亜鉛粒子は、亜鉛化合物とアンモニウムイオンを含む水溶液を加熱して塩基性炭酸亜鉛の沈殿物を得たのち、得られた塩基性炭酸亜鉛を焼成、粉砕及び噴霧乾燥することにより製造することができる。
一般に、粉砕、噴霧条件、焼成条件を適宜変更することにより、粒子形状、粒子径、比表面積、細孔径を調節することができる。 <Method for producing zinc oxide particles>
The zinc oxide particles having the above-described shape and physical properties can be produced by heating an aqueous solution containing a zinc compound and ammonium ions to obtain a precipitate of basic zinc carbonate, and then firing, pulverizing, and spray-drying the obtained basic zinc carbonate.
In general, the particle shape, particle size, specific surface area and pore size can be adjusted by appropriately changing the pulverization, spraying conditions and firing conditions.
上記の形状及び物性を有する酸化亜鉛粒子は、亜鉛化合物とアンモニウムイオンを含む水溶液を加熱して塩基性炭酸亜鉛の沈殿物を得たのち、得られた塩基性炭酸亜鉛を焼成、粉砕及び噴霧乾燥することにより製造することができる。
一般に、粉砕、噴霧条件、焼成条件を適宜変更することにより、粒子形状、粒子径、比表面積、細孔径を調節することができる。 <Method for producing zinc oxide particles>
The zinc oxide particles having the above-described shape and physical properties can be produced by heating an aqueous solution containing a zinc compound and ammonium ions to obtain a precipitate of basic zinc carbonate, and then firing, pulverizing, and spray-drying the obtained basic zinc carbonate.
In general, the particle shape, particle size, specific surface area and pore size can be adjusted by appropriately changing the pulverization, spraying conditions and firing conditions.
＜酸化亜鉛粒子の含有量＞
本発明の化粧料における酸化亜鉛粒子の含有量は、特に制限されないが、下限としては、１．０質量％以上が好ましく、さらに好ましくは５．０質量％以上であり、特に好ましくは１０．０質量％以上である。上限としては、５０．０質量％以下が好ましく、さらに好ましくは３０質量％以下であり、特に好ましくは２０．０質量％以下である。よって、酸化亜鉛粒子の含有量の範囲としては、例えば１０．０～２０．０質量％等が挙げられる。化粧料における酸化亜鉛粒子の含有量を上記範囲とすることで、使用感触を損なうことなく、皮脂を十分に固化し、高い化粧崩れ防止効果を発揮することができる。 <Content of zinc oxide particles>
The content of zinc oxide particles in the cosmetic of the present invention is not particularly limited, but the lower limit is preferably 1.0% by mass or more, more preferably 5.0% by mass or more, and particularly preferably 10.0% by mass or more. The upper limit is preferably 50.0% by mass or less, more preferably 30% by mass or less, and particularly preferably 20.0% by mass or less. Therefore, the content range of the zinc oxide particles is, for example, 10.0 to 20.0% by mass. By setting the content of the zinc oxide particles in the cosmetic in the above range, it is possible to sufficiently solidify sebum without impairing the feeling of use, and exhibit a high effect of preventing makeup deterioration.
本発明の化粧料における酸化亜鉛粒子の含有量は、特に制限されないが、下限としては、１．０質量％以上が好ましく、さらに好ましくは５．０質量％以上であり、特に好ましくは１０．０質量％以上である。上限としては、５０．０質量％以下が好ましく、さらに好ましくは３０質量％以下であり、特に好ましくは２０．０質量％以下である。よって、酸化亜鉛粒子の含有量の範囲としては、例えば１０．０～２０．０質量％等が挙げられる。化粧料における酸化亜鉛粒子の含有量を上記範囲とすることで、使用感触を損なうことなく、皮脂を十分に固化し、高い化粧崩れ防止効果を発揮することができる。 <Content of zinc oxide particles>
The content of zinc oxide particles in the cosmetic of the present invention is not particularly limited, but the lower limit is preferably 1.0% by mass or more, more preferably 5.0% by mass or more, and particularly preferably 10.0% by mass or more. The upper limit is preferably 50.0% by mass or less, more preferably 30% by mass or less, and particularly preferably 20.0% by mass or less. Therefore, the content range of the zinc oxide particles is, for example, 10.0 to 20.0% by mass. By setting the content of the zinc oxide particles in the cosmetic in the above range, it is possible to sufficiently solidify sebum without impairing the feeling of use, and exhibit a high effect of preventing makeup deterioration.
＜酸化亜鉛粒子を含む化粧料＞
本発明の化粧料としては、特に制限されず、洗顔クリーム、化粧水、マッサージクリーム、乳液、モイスチャークリームなどのスキンケア化粧品、ファンデーション、フェイスパウダー、化粧下地、おしろい、アイシャドウ、アイライナー、口紅、ほほ紅などのメイクアップ化粧料、入浴剤、日焼け止めクリーム、デオドラントスプレーなどのボディケア化粧品、シャンプー、リンス、ヘアリキッド、ヘアカラーなどのヘアケア化粧品など、一般的な化粧料が挙げられるが、メイクアップ化粧料、なかでもファンデーション、フェイスパウダー、化粧下地、おしろいに配合されることで優れた効果を発揮できる。 <Cosmetics containing zinc oxide particles>
The cosmetic of the present invention is not particularly limited, and includes general cosmetics such as skin care cosmetics such as face wash cream, lotion, massage cream, milky lotion, and moisture cream; makeup cosmetics such as foundation, face powder, makeup base, face powder, eye shadow, eyeliner, lipstick, and blush; body care cosmetics such as bath salts, sunscreen creams, and deodorant sprays; Excellent effects can be exhibited by being blended into makeup bases, face powders, makeup bases, and face powders.
本発明の化粧料としては、特に制限されず、洗顔クリーム、化粧水、マッサージクリーム、乳液、モイスチャークリームなどのスキンケア化粧品、ファンデーション、フェイスパウダー、化粧下地、おしろい、アイシャドウ、アイライナー、口紅、ほほ紅などのメイクアップ化粧料、入浴剤、日焼け止めクリーム、デオドラントスプレーなどのボディケア化粧品、シャンプー、リンス、ヘアリキッド、ヘアカラーなどのヘアケア化粧品など、一般的な化粧料が挙げられるが、メイクアップ化粧料、なかでもファンデーション、フェイスパウダー、化粧下地、おしろいに配合されることで優れた効果を発揮できる。 <Cosmetics containing zinc oxide particles>
The cosmetic of the present invention is not particularly limited, and includes general cosmetics such as skin care cosmetics such as face wash cream, lotion, massage cream, milky lotion, and moisture cream; makeup cosmetics such as foundation, face powder, makeup base, face powder, eye shadow, eyeliner, lipstick, and blush; body care cosmetics such as bath salts, sunscreen creams, and deodorant sprays; Excellent effects can be exhibited by being blended into makeup bases, face powders, makeup bases, and face powders.
本発明の化粧料は、用途に応じて、化粧品に通常使用される他の成分を含有することができる。主なものとして、粉末、油分、水性成分が挙げられ、そのほかにも例えば、水溶性高分子化合物、増粘剤、紫外線吸収剤、金属イオン封鎖剤、アミノ酸類、皮膚栄養剤、血行促進剤、制汗剤、殺菌剤、消炎剤、酸化防止剤、防腐剤、香料等を添加することができる。
The cosmetic composition of the present invention can contain other ingredients that are commonly used in cosmetics, depending on the application. Main examples include powders, oils, and aqueous components. In addition, water-soluble polymer compounds, thickeners, ultraviolet absorbers, sequestering agents, amino acids, skin nutrients, blood circulation promoters, antiperspirants, bactericides, antiphlogistic agents, antioxidants, preservatives, fragrances, and the like can be added.
本発明の化粧料に配合できる粉末は、特に限定はされないが、例えば、タルク、セリサイト、マイカ、カオリン、炭酸マグネシウム、炭酸カルシウム、ケイ酸アルミニウム、ケイ酸バリウム、ケイ酸カルシウム、ケイ酸マグネシウム、ケイ酸ストロンチウム、タングステン酸金属塩、マグネシウム、シリカ、ゼオライト、硫酸バリウム、焼成硫酸カルシウム、リン酸カルシウム、フッ素アパタイト、ヒドロキシアパタイト、金属石鹸、窒化ホウ素、ナイロンパウダー、ポリエチレンパウダー、セルロースパウダー、シリコーン系粉末、亜鉛華等の体質顔料；カーボンブラック、酸化チタン、群青、紺青、酸化クロム、有機タール系色素、レーキ等の着色剤；雲母チタン、酸化鉄コーテッド雲母等の複合顔料；これらの粉末をシリコーン化合物、フッ素変性シリコーン化合物、フッ素化合物、高級脂肪酸、高級アルコール、脂肪酸エステル、金属石鹸、アミノ酸、４級アンモニウム塩、アルキルホスフェート等により疎水化処理したもの等が含まれる。
The powder that can be blended in the cosmetic of the present invention is not particularly limited, but for example, talc, sericite, mica, kaolin, magnesium carbonate, calcium carbonate, aluminum silicate, barium silicate, calcium silicate, magnesium silicate, strontium silicate, metal tungstate, magnesium, silica, zeolite, barium sulfate, calcined calcium sulfate, calcium phosphate, fluoroapatite, hydroxyapatite, metallic soap, boron nitride, nylon powder, polyethylene powder, cellulose powder, silicone powder, zinc oxide. Extender pigments such as carbon black, titanium oxide, ultramarine blue, Prussian blue, chromium oxide, organic tar pigments, lakes, and other coloring agents; mica titanium, iron oxide-coated mica and other composite pigments; silicone compounds, fluorine-modified silicone compounds, fluorine compounds, higher fatty acids, higher alcohols, fatty acid esters, metal soaps, amino acids, quaternary ammonium salts, alkyl phosphates, and the like.
本発明の化粧料に配合できる油分は、一般的な化粧料に用いられ得るものであれば特に限定されるものではなく、炭化水素油、合成エステル油、シリコーン油等が挙げられる。使用性および使用感等の観点から、シリコーン油を含むことが好ましい。
The oil that can be blended in the cosmetic of the present invention is not particularly limited as long as it can be used in general cosmetics, and includes hydrocarbon oil, synthetic ester oil, silicone oil, and the like. From the viewpoints of usability, feeling of use, etc., it is preferable that silicone oil is included.
本発明の化粧料に配合できる水性成分は、水に可溶な成分であれば特に制約なく使用することができる。水性成分としては、例えば、エチルアルコール等の低級アルコール類等のほか、キレート剤、ｐＨ調整剤、防腐剤等も挙げられる。
Aqueous components that can be blended in the cosmetics of the present invention can be used without any particular restrictions as long as they are water-soluble components. Examples of aqueous components include lower alcohols such as ethyl alcohol, chelating agents, pH adjusters, preservatives, and the like.
以下に実施例を挙げて本発明をさらに詳述するが、本発明はこれらにより何ら限定されるものではない。配合量は特記しない限り、その成分が配合される系に対する質量％で示す。各実施例について具体的に説明する前に、採用した評価方法について説明する。
The present invention will be described in more detail below with reference to examples, but the present invention is not limited by these. Unless otherwise specified, the blending amount is shown in % by mass relative to the system in which the component is blended. Before describing each example in detail, the employed evaluation method will be described.
＜形状＞
走査型電子顕微鏡で観察することにより、粒子の形状と粒子径を確認した。
＜メディアン径（Ｄ５０）＞
（株）島津製作所製、ＳＡＬＤ－７１００を使用して、酸化亜鉛粒子の各試料について粒度分布を求め、積算値が５０％に相当する粒径を調べた。 <Shape>
The particle shape and particle size were confirmed by observation with a scanning electron microscope.
<Median diameter (D50)>
Using SALD-7100 manufactured by Shimadzu Corporation, the particle size distribution was obtained for each sample of zinc oxide particles, and the particle size corresponding to the integrated value of 50% was examined.
走査型電子顕微鏡で観察することにより、粒子の形状と粒子径を確認した。
＜メディアン径（Ｄ５０）＞
（株）島津製作所製、ＳＡＬＤ－７１００を使用して、酸化亜鉛粒子の各試料について粒度分布を求め、積算値が５０％に相当する粒径を調べた。 <Shape>
The particle shape and particle size were confirmed by observation with a scanning electron microscope.
<Median diameter (D50)>
Using SALD-7100 manufactured by Shimadzu Corporation, the particle size distribution was obtained for each sample of zinc oxide particles, and the particle size corresponding to the integrated value of 50% was examined.
＜ＢＥＴ比表面積＞
ＢＥＴ比表面積を、マイクロトラック・ベル株式会社製、ＢＥＬＳＯＲＰ－ｍｉｎｉＩＩを使用して測定した。 <BET specific surface area>
The BET specific surface area was measured using BELSORP-miniII manufactured by Microtrack Bell Co., Ltd.
ＢＥＴ比表面積を、マイクロトラック・ベル株式会社製、ＢＥＬＳＯＲＰ－ｍｉｎｉＩＩを使用して測定した。 <BET specific surface area>
The BET specific surface area was measured using BELSORP-miniII manufactured by Microtrack Bell Co., Ltd.
＜細孔径ピーク＞
酸化亜鉛粒子の各試料について、ガス吸着方式による細孔分布測定装置を用いて、各圧力における窒素ガスの吸着量を求め、ＢＪＨ法で計算された累積細孔体積分布及び細孔分布を得た。分布から細孔径ピークをそれぞれ求めた。 <Pore size peak>
For each sample of zinc oxide particles, the amount of nitrogen gas adsorbed at each pressure was determined using a gas adsorption type pore distribution measuring device, and the cumulative pore volume distribution and pore distribution calculated by the BJH method were obtained. A pore size peak was determined from the distribution.
酸化亜鉛粒子の各試料について、ガス吸着方式による細孔分布測定装置を用いて、各圧力における窒素ガスの吸着量を求め、ＢＪＨ法で計算された累積細孔体積分布及び細孔分布を得た。分布から細孔径ピークをそれぞれ求めた。 <Pore size peak>
For each sample of zinc oxide particles, the amount of nitrogen gas adsorbed at each pressure was determined using a gas adsorption type pore distribution measuring device, and the cumulative pore volume distribution and pore distribution calculated by the BJH method were obtained. A pore size peak was determined from the distribution.
＜皮脂固化効果＞
室温において、２０ｍＬのスクリュー管に酸化亜鉛粒子試料０．２ｇ、オレイン酸９．８ｇを入れ、手で３０秒間振り混ぜた。振り混ぜた直後、３７℃の恒温槽で１５分静置後、３０分静置後、２時間静置後及びその後さらに室温で１２時間静置後の固化の状態を以下の基準に従って評価した。
Ａ：オレイン酸が固化しスクリュー管を傾けても流れない。また、液状物の存在が確認できない。
Ｂ：オレイン酸が固化しスクリュー管を傾けても流れないが、一部のオレイン酸が液状のまま残存している。
Ｃ：オレイン酸はほぼ固化しているが柔らかいためスクリュー管を傾けると若干流れる。
Ｄ：オレイン酸が固化せず、スクリュー管を傾けると流れる。 <Sebum solidification effect>
At room temperature, 0.2 g of a zinc oxide particle sample and 9.8 g of oleic acid were placed in a 20 mL screw tube and shaken by hand for 30 seconds. Immediately after shaking and mixing, after standing in a constant temperature bath at 37° C. for 15 minutes, after standing for 30 minutes, after standing for 2 hours, and after standing at room temperature for 12 hours, the state of solidification was evaluated according to the following criteria.
A: Oleic acid solidifies and does not flow even when the screw tube is tilted. In addition, the presence of liquid matter cannot be confirmed.
B: Oleic acid solidified and did not flow even when the screw tube was tilted, but some oleic acid remained in a liquid state.
C: Oleic acid is almost solidified, but since it is soft, it flows slightly when the screw tube is tilted.
D: Oleic acid did not solidify and flowed when the screw tube was tilted.
室温において、２０ｍＬのスクリュー管に酸化亜鉛粒子試料０．２ｇ、オレイン酸９．８ｇを入れ、手で３０秒間振り混ぜた。振り混ぜた直後、３７℃の恒温槽で１５分静置後、３０分静置後、２時間静置後及びその後さらに室温で１２時間静置後の固化の状態を以下の基準に従って評価した。
Ａ：オレイン酸が固化しスクリュー管を傾けても流れない。また、液状物の存在が確認できない。
Ｂ：オレイン酸が固化しスクリュー管を傾けても流れないが、一部のオレイン酸が液状のまま残存している。
Ｃ：オレイン酸はほぼ固化しているが柔らかいためスクリュー管を傾けると若干流れる。
Ｄ：オレイン酸が固化せず、スクリュー管を傾けると流れる。 <Sebum solidification effect>
At room temperature, 0.2 g of a zinc oxide particle sample and 9.8 g of oleic acid were placed in a 20 mL screw tube and shaken by hand for 30 seconds. Immediately after shaking and mixing, after standing in a constant temperature bath at 37° C. for 15 minutes, after standing for 30 minutes, after standing for 2 hours, and after standing at room temperature for 12 hours, the state of solidification was evaluated according to the following criteria.
A: Oleic acid solidifies and does not flow even when the screw tube is tilted. In addition, the presence of liquid matter cannot be confirmed.
B: Oleic acid solidified and did not flow even when the screw tube was tilted, but some oleic acid remained in a liquid state.
C: Oleic acid is almost solidified, but since it is soft, it flows slightly when the screw tube is tilted.
D: Oleic acid did not solidify and flowed when the screw tube was tilted.
＜使用感触＞
以下の組成を有する粉末化粧料（ファンデーション）を、酸化亜鉛粒子の試料ごとに調製した。具体的には、下記成分をヘンシェルミキサーで混合し、パルペライザーで解砕した後、樹脂製の中皿容器に充填し、公知の方法で乾式プレス成型を行なって、粉末化粧料を得た。
ファンデーション
（成分名） 配合量（質量％）
タルク 残部
酸化亜鉛粒子（試料１～１８のいずれか） ５
雲母 ２０
酸化チタン １０
ジメチコン ２５
メチルフェニルポリシロキサン ５ <feel of use>
A powder cosmetic (foundation) having the following composition was prepared for each sample of zinc oxide particles. Specifically, the following components were mixed in a Henschel mixer, pulverized in a pulperizer, filled in a resin-made medium dish container, and dry-pressed by a known method to obtain a powdered cosmetic.
Foundation (ingredient name) Amount (% by mass)
Talc Balance zinc oxide particles (any of samples 1 to 18) 5
mica 20
Titanium oxide 10
Dimethicone 25
Methylphenylpolysiloxane 5
以下の組成を有する粉末化粧料（ファンデーション）を、酸化亜鉛粒子の試料ごとに調製した。具体的には、下記成分をヘンシェルミキサーで混合し、パルペライザーで解砕した後、樹脂製の中皿容器に充填し、公知の方法で乾式プレス成型を行なって、粉末化粧料を得た。
ファンデーション
（成分名） 配合量（質量％）
タルク 残部
酸化亜鉛粒子（試料１～１８のいずれか） ５
雲母 ２０
酸化チタン １０
ジメチコン ２５
メチルフェニルポリシロキサン ５ <feel of use>
A powder cosmetic (foundation) having the following composition was prepared for each sample of zinc oxide particles. Specifically, the following components were mixed in a Henschel mixer, pulverized in a pulperizer, filled in a resin-made medium dish container, and dry-pressed by a known method to obtain a powdered cosmetic.
Foundation (ingredient name) Amount (% by mass)
Talc Balance zinc oxide particles (any of samples 1 to 18) 5
mica 20
Titanium oxide 10
Dimethicone 25
Methylphenylpolysiloxane 5
得られた粉末化粧料について、肌に塗布した際の使用感触（滑らかさ、きしみ感の無さ）を以下の方法で評価した。
化粧品評価専門パネル２０名に粉末化粧料を使用してもらい、使用感触を以下の基準に従って５段階評価し、化粧料毎に評点を付し、さらに全パネルの評点の平均点を以下の４段階の判断基準に従って判定した。
（評価基準）
評価結果 ： 評点
非常に良好 ： ５点
良好 ： ４点
普通 ： ３点
やや不良 ： ２点
不良 ： １点
（判定基準）
判定 ： 評点の平均点
Ａ ： ４．５以上
Ｂ ： ３．５以上～４．５未満
Ｃ ： １．５以上～３．５未満
Ｄ ： １．５未満 The resulting powdery cosmetic was evaluated for feel in use (smoothness, absence of squeaky feeling) when applied to the skin by the following methods.
A panel of 20 cosmetics evaluation specialists used the powdered cosmetics, evaluated the feeling of use in five stages according to the following criteria, assigned a score to each cosmetic, and further evaluated the average score of all the panels according to the following four-stage judgment criteria.
(Evaluation criteria)
Evaluation results: Very good: 5 points Good: 4 points Average: 3 points Somewhat poor: 2 points Poor: 1 point (judgment criteria)
Judgment: Average score A: 4.5 or more B: 3.5 or more to less than 4.5 C: 1.5 or more to less than 3.5 D: less than 1.5
化粧品評価専門パネル２０名に粉末化粧料を使用してもらい、使用感触を以下の基準に従って５段階評価し、化粧料毎に評点を付し、さらに全パネルの評点の平均点を以下の４段階の判断基準に従って判定した。
（評価基準）
評価結果 ： 評点
非常に良好 ： ５点
良好 ： ４点
普通 ： ３点
やや不良 ： ２点
不良 ： １点
（判定基準）
判定 ： 評点の平均点
Ａ ： ４．５以上
Ｂ ： ３．５以上～４．５未満
Ｃ ： １．５以上～３．５未満
Ｄ ： １．５未満 The resulting powdery cosmetic was evaluated for feel in use (smoothness, absence of squeaky feeling) when applied to the skin by the following methods.
A panel of 20 cosmetics evaluation specialists used the powdered cosmetics, evaluated the feeling of use in five stages according to the following criteria, assigned a score to each cosmetic, and further evaluated the average score of all the panels according to the following four-stage judgment criteria.
(Evaluation criteria)
Evaluation results: Very good: 5 points Good: 4 points Average: 3 points Somewhat poor: 2 points Poor: 1 point (judgment criteria)
Judgment: Average score A: 4.5 or more B: 3.5 or more to less than 4.5 C: 1.5 or more to less than 3.5 D: less than 1.5
表１に示されるように、メディアン径（Ｄ５０）が１～３００μｍ、ＢＥＴ比表面積が２０ｍ２／ｇ以上であって、なおかつ、球状である酸化亜鉛粒子は、十分な皮脂固化効果を有するとともに、化粧料に配合した際に優れた使用感触を示した（試料１～１０）。なかでも、ＢＥＴ比表面積が１１０～１３０ｍ２／ｇであるものは、振り混ぜた直後から優れた皮脂固化効果を発揮することが確認された（試料２～５）。
また、一般的には、ＢＥＴ比表面積が大きい方が皮脂との接触面が増えるため、酸化亜鉛と反応しやすくなり高い皮脂固化効果を示すと考えられるが、必ずしもそのような結果を示さないことが確認された（試料６）。 As shown in Table 1, the spherical zinc oxide particles having a median diameter (D50) of 1 to 300 μm, a BET specific surface area of 20 m 2 /g or more, and having a sufficient sebum-solidifying effect, exhibited an excellent feel during use when blended in cosmetics (Samples 1 to 10). Among them, it was confirmed that those having a BET specific surface area of 110 to 130 m 2 /g exhibited an excellent sebum-solidifying effect immediately after being shaken (Samples 2 to 5).
Also, in general, the larger the BET specific surface area, the more the contact surface with sebum, so it is thought that it is likely to react with zinc oxide and exhibit a high sebum-solidifying effect, but it was confirmed that such a result was not necessarily shown (Sample 6).
また、一般的には、ＢＥＴ比表面積が大きい方が皮脂との接触面が増えるため、酸化亜鉛と反応しやすくなり高い皮脂固化効果を示すと考えられるが、必ずしもそのような結果を示さないことが確認された（試料６）。 As shown in Table 1, the spherical zinc oxide particles having a median diameter (D50) of 1 to 300 μm, a BET specific surface area of 20 m 2 /g or more, and having a sufficient sebum-solidifying effect, exhibited an excellent feel during use when blended in cosmetics (Samples 1 to 10). Among them, it was confirmed that those having a BET specific surface area of 110 to 130 m 2 /g exhibited an excellent sebum-solidifying effect immediately after being shaken (Samples 2 to 5).
Also, in general, the larger the BET specific surface area, the more the contact surface with sebum, so it is thought that it is likely to react with zinc oxide and exhibit a high sebum-solidifying effect, but it was confirmed that such a result was not necessarily shown (Sample 6).
一方、形状が不定形や板状のもの、及び粒子径が１μｍ以下の小さい粒子は、使用感触が著しく劣っていた（試料１１～１７）。また、ＢＥＴ比表面積が２０ｍ２／ｇ未満の場合は皮脂固化効果が不十分であった（試料１７及び１８）。
On the other hand, irregular or plate-like particles and small particles with a particle diameter of 1 μm or less had a significantly inferior feeling in use (Samples 11 to 17). Moreover, when the BET specific surface area was less than 20 m 2 /g, the sebum-solidifying effect was insufficient (Samples 17 and 18).
Claims (5)
- メディアン径（Ｄ５０）が１～３００μｍであり、かつ、ＢＥＴ比表面積が２０ｍ２／ｇ以上である、球状の酸化亜鉛粒子を含有する化粧料。 A cosmetic containing spherical zinc oxide particles having a median diameter (D50) of 1 to 300 μm and a BET specific surface area of 20 m 2 /g or more.
- 酸化亜鉛粒子のＢＥＴ比表面積が１１０～１３０ｍ２／ｇである、請求項１に記載の化粧料。 The cosmetic according to claim 1, wherein the zinc oxide particles have a BET specific surface area of 110 to 130 m 2 /g.
- 酸化亜鉛粒子の細孔径ピークが７ｎｍ以上である、請求項１に記載の化粧料。 The cosmetic according to claim 1, wherein the zinc oxide particles have a pore size peak of 7 nm or more.
- 酸化亜鉛粒子が皮脂固化剤である、請求項１に記載の化粧料。 The cosmetic according to Claim 1, wherein the zinc oxide particles are a sebum solidifying agent.
- メイクアップ化粧料である、請求項１に記載の化粧料。 The cosmetic according to Claim 1, which is a make-up cosmetic.
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| WO2016190399A1 (en) * | 2015-05-28 | 2016-12-01 | 堺化学工業株式会社 | Sebum adsorbent and cosmetic comprising same |
| JP2018083765A (en) * | 2016-11-21 | 2018-05-31 | 堺化学工業株式会社 | Unsaturated fatty acid adsorbent and cosmetic containing the same |
| JP2020019720A (en) * | 2018-07-30 | 2020-02-06 | 株式会社ファンケル | Plate-like zinc oxide powder and cosmetic containing the same |
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