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JP7436967B2 - Spherical composite powder for cosmetics and method for producing the same - Google Patents
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JP7436967B2 - Spherical composite powder for cosmetics and method for producing the same - Google Patents

Spherical composite powder for cosmetics and method for producing the same Download PDF

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JP7436967B2
JP7436967B2 JP2019124150A JP2019124150A JP7436967B2 JP 7436967 B2 JP7436967 B2 JP 7436967B2 JP 2019124150 A JP2019124150 A JP 2019124150A JP 2019124150 A JP2019124150 A JP 2019124150A JP 7436967 B2 JP7436967 B2 JP 7436967B2
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spherical composite
composite powder
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直晃 豊田
俊彦 岡寺
浩志 浅野
泰正 高尾
巌 浅井
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National Institute of Advanced Industrial Science and Technology AIST
Nippon Menard Cosmetic Co Ltd
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Nippon Menard Cosmetic Co Ltd
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Description

本願発明は、球形性が高く、柔らかい感触特性を有する環境適合性の化粧料用球状複合粉体、及びその製造方法に関する。 The present invention relates to an environmentally compatible spherical composite powder for cosmetics that has high sphericity and soft touch characteristics, and a method for producing the same.

近年、プラスチックごみの海洋流出に伴う環境、及び生態系への悪影響が表面化し、世界的に関心が寄せられている(非特許文献1)。特に粒子径5mm以下の合成ポリマー粒子は、通称プラスチックマイクロビーズ(以下PMB)と呼称され、各国で規制対象となりつつある。 In recent years, the negative impact on the environment and ecosystem caused by the outflow of plastic waste into the ocean has come to the fore and has attracted worldwide attention (Non-Patent Document 1). In particular, synthetic polymer particles with a particle diameter of 5 mm or less are commonly referred to as plastic microbeads (hereinafter referred to as PMB), and are becoming subject to regulations in many countries.

化粧品分野においては、洗顔料等に配合されるスクラブ剤(メディアン径数百μmのPMB)がまず規制対象とされ、国内各社でセルロース等の天然由来粒子へと代替されている(非特許文献2)。 In the field of cosmetics, scrubbing agents (PMB with a median diameter of several hundred μm) that are incorporated into facial cleansers etc. were first subject to regulation, and domestic companies are replacing them with naturally derived particles such as cellulose (Non-patent Document 2). ).

一方、プレストファンデーション(以下PF)には、感触改良を目的としてメディアン径10μm前後のナイロンやポリウレタンといった合成ポリマーからなる球状粉体が含有される。このPMBは、独特の転がり性や柔らかさを有することから、PF製剤の感触特性に及ぼす影響は大きく、他の原料への代替が非常に難しいという現状がある。 On the other hand, pressed foundation (hereinafter referred to as PF) contains spherical powder made of synthetic polymer such as nylon or polyurethane with a median diameter of about 10 μm for the purpose of improving the feel. Since this PMB has unique rolling properties and softness, it has a large influence on the tactile characteristics of PF formulations, and it is currently very difficult to substitute it with other raw materials.

PFに含有されるPMBの代替候補原料としては、球状シリカや球状セルロースが挙げられる。粒子形態制御によって多孔質構造を有する球状セルロースが開示されている(特許文献1、2)。しかしながら、いずれも上記合成ポリマーと比較して感触は硬く、代替原料として満足できるものではなかった。 Spherical silica and spherical cellulose are examples of alternative raw materials for PMB contained in PF. Spherical cellulose having a porous structure through particle morphology control has been disclosed (Patent Documents 1 and 2). However, all of them had a harder feel than the above synthetic polymers and were not satisfactory as alternative raw materials.

このような背景のもと、環境適合性で、かつ感触の柔らかい従来の合成ポリマー(PMB)に代替しうる化粧料用球状粉体の開発が潜在的に望まれている。 Against this background, there is a potential desire to develop a spherical powder for cosmetics that is environmentally compatible and soft to the touch and can replace conventional synthetic polymers (PMB).

特開1994-136175号公報Japanese Patent Application Publication No. 1994-136175 特開1985-197746号公報Japanese Patent Application Publication No. 1985-197746

甲子園大学紀要 No.45、p37-44(2018) プラスチックによる海洋汚染の現状と課題、とくにマイクロプラスチックについてKoshien University Bulletin No. 45, p37-44 (2018) Current status and challenges of marine pollution caused by plastics, especially regarding microplastics 日本化粧品工業連合会自主基準通知文書 2016年3月17日発表 洗い流しのスクラブ製品におけるマイクロプラスチックビーズの使用についてJapan Cosmetic Industry Federation Voluntary Standards Notification Document Announced on March 17, 2016 Regarding the use of microplastic beads in wash-off scrub products

本願発明は、上記事情に鑑みてなされたもので、球形性が高く、感触の柔らかい環境適合性の化粧料用球状複合粉体、及びその製造方法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 aims to provide a spherical composite powder for cosmetics that has high sphericity, is soft to the touch, and is environmentally compatible, and a method for producing the same.

かかる実情において、本願発明者らは上記課題を解決すべく鋭意研究を重ねた結果、特定の鉱物、及び水溶性多糖類から構成される凝集粒子が、球形性が高く、感触の柔らかい化粧料用球状複合粉体として利用でき、従来の合成ポリマー(PMB)に代替しうる感触特性を有することを見出し、本願発明を完成するに至った。 Under these circumstances, the inventors of the present application have conducted extensive research to solve the above problems, and have found that aggregate particles composed of specific minerals and water-soluble polysaccharides are highly spherical and have a soft texture for use in cosmetics. It was discovered that it can be used as a spherical composite powder and has tactile properties that can be used as a substitute for conventional synthetic polymers (PMB), leading to the completion of the present invention.

本願発明は、特定のメディアン径を有する鉱物と、水溶性多糖類とを含有することを特徴とする化粧料用球状複合粉体と、その製造方法を提供するものである。 The present invention provides a spherical composite powder for cosmetics, which is characterized by containing a mineral having a specific median diameter and a water-soluble polysaccharide, and a method for producing the same.

本願発明は、球形性が高く、感触の柔らかい環境適合性の化粧料用球状複合粉体、及びその製造方法を提供するものである。 The present invention provides a spherical composite powder for cosmetics that has high sphericity, is soft to the touch, and is environmentally compatible, and a method for producing the same.

実施例1で得られた化粧料用球状複合粉体の電子顕微鏡像Electron microscope image of the spherical composite powder for cosmetics obtained in Example 1

以下本願発明の、球形性が高く、感触の柔らかい環境適合性の化粧料用球状複合粉体、及びその製造方法を、その好ましい実施形態に基づいて説明する。本願発明によれば、感触の柔らかい従来の合成ポリマー(PMB)に代替しうる化粧料用球状複合粉体を得ることができる。 DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The spherical composite powder for cosmetics, which has high sphericity, is soft to the touch, and is environmentally compatible, and the method for producing the same, according to the present invention, will be described below based on preferred embodiments thereof. According to the present invention, it is possible to obtain a spherical composite powder for cosmetics that can replace a conventional synthetic polymer (PMB) that is soft to the touch.

本願発明の構成成分(A)は、Si、Al、Mg、及びKのうち2種類以上を構成元素とする天然鉱物、あるいは合成鉱物であり、通常、化粧料に用いられる鉱物であれば特に限定されない。例えば、構成元素としてSi、Mgを含有するタルク、構成元素としてSi、Al、Kを含有するセリサイト、構成元素としてSi、Alを含有するカオリン等が挙げられる。 The component (A) of the present invention is a natural mineral or a synthetic mineral containing two or more of Si, Al, Mg, and K as constituent elements, and is particularly limited if it is a mineral that is normally used in cosmetics. Not done. Examples include talc containing Si and Mg as constituent elements, sericite containing Si, Al, and K as constituent elements, and kaolin containing Si and Al as constituent elements.

本願発明の構成成分(A)のメディアン径は、0.5~2.1μmである。より好ましくは0.6~1.5μmである。2.1μmよりも大きいと、得られる化粧料用球状複合粉体の球形性が低下する。0.5μm以上であれば、良好な球形性を有する化粧料用球状複合粉体を得ることができる。 The median diameter of the component (A) of the present invention is 0.5 to 2.1 μm. More preferably, it is 0.6 to 1.5 μm. If it is larger than 2.1 μm, the sphericity of the resulting spherical composite powder for cosmetics will decrease. If it is 0.5 μm or more, a spherical composite powder for cosmetics having good sphericity can be obtained.

本願発明の構成成分(A)のメディアン径は、汎用の粒度分布測定装置によって特定することができる。例えば、レーザー回折方式、光散乱方式、画像解析方式のいずれを用いても良い。これらの中で、本願発明の粒子径範囲を測定することを考慮すると、レーザー回折方式が好ましく、具体的には、Partica LA-950V2(HORIBA社製)等を用いてメディアン径を測定することができる。 The median diameter of the component (A) of the present invention can be determined using a general-purpose particle size distribution measuring device. For example, any of a laser diffraction method, a light scattering method, and an image analysis method may be used. Among these, in consideration of measuring the particle size range of the present invention, the laser diffraction method is preferable, and specifically, it is possible to measure the median diameter using Partica LA-950V2 (manufactured by HORIBA) or the like. can.

本願発明の構成成分(A)としては、市販品を用いることができる。例えば、ナノエース D-600(成分:タルク、メディアン径:0.6μm、日本タルク社製)や、ナノエース D-1000F(成分:タルク、メディアン径1.0μm:日本タルク社製)等を用いることができる。また、目的とするメディアン径を有する鉱物を得るために、2.1μmよりも大きいメディアン径の鉱物に機械的粉砕処理を加えて別途調製しても良い。 As the component (A) of the present invention, commercially available products can be used. For example, Nano Ace D-600 (component: talc, median diameter: 0.6 μm, manufactured by Nippon Talc Co., Ltd.), Nano Ace D-1000F (component: talc, median diameter: 1.0 μm, manufactured by Nippon Talc Co., Ltd.), etc. can be used. can. Further, in order to obtain a mineral having a desired median diameter, a mineral having a median diameter larger than 2.1 μm may be separately prepared by subjecting it to a mechanical crushing process.

本願発明で用いる構成成分(A)の物理特性として、さらに重要なのは、構成成分(A)の分散状態の指標となるせん断粘度である。分散状態により球状複合粉体の球形性が変化する。本願発明では、構成成分(A)の40重量%水分散体をE型粘度計で測定したときに得られるせん断粘度(せん断速度10/sec)は、100mPa・s以上である。より好ましくは1,000mPa・s以上、最も好ましくは10,000mPa・s以上である。40重量%水分散体のせん断粘度が100mPa・sよりも小さい天然鉱物、あるいは合成鉱物では、得られる化粧料用球状複合粉体の球形性が低下する恐れがある。40重量%水分散体のせん断粘度が100mPa・s以上の天然鉱物、あるいは合成鉱物であれば、球形性の良好な化粧料用球状複合粉体を得ることができる。 What is more important as a physical property of the component (A) used in the present invention is the shear viscosity, which is an index of the dispersion state of the component (A). The sphericity of the spherical composite powder changes depending on the state of dispersion. In the present invention, the shear viscosity (shear rate 10/sec) obtained when a 40% by weight aqueous dispersion of component (A) is measured with an E-type viscometer is 100 mPa·s or more. More preferably, it is 1,000 mPa·s or more, most preferably 10,000 mPa·s or more. If the shear viscosity of the 40% by weight aqueous dispersion is less than 100 mPa·s, natural minerals or synthetic minerals may reduce the sphericity of the resulting spherical composite powder for cosmetics. A spherical composite powder for cosmetics with good sphericity can be obtained if the 40% by weight water dispersion is a natural mineral or a synthetic mineral with a shear viscosity of 100 mPa·s or more.

本願発明の化粧料用球状複合粉体を構成する天然鉱物、あるいは合成鉱物の40重量%水分散体のせん断粘度は、汎用のE型粘度計を用いて一定せん断速度下でのせん断粘度として特定することができる。具体的には、Physica MCR 301(アントンパール社製)を用いてせん断粘度を測定することができる。 The shear viscosity of the 40% by weight aqueous dispersion of natural minerals or synthetic minerals constituting the spherical composite powder for cosmetics of the present invention is determined as the shear viscosity under a constant shear rate using a general-purpose E-type viscometer. can do. Specifically, the shear viscosity can be measured using Physica MCR 301 (manufactured by Anton Paar).

上記物理的特性を考慮すると、本願発明の構成成分(A)として、より好ましくはタルク、カオリンであり、最も好ましくはタルクである。 Considering the above physical properties, the component (A) of the present invention is more preferably talc or kaolin, and most preferably talc.

本願発明の構成成分(B)水溶性多糖類は、通常、化粧料に用いられる水溶性多糖類であれば特に限定されない。具体的には、例えば、澱粉、水溶性セルロース誘導体、及びその塩等が挙げられる。澱粉としては、例えば、米澱粉、小麦澱粉、コーンスターチ等の種実澱粉や、タピオカ澱粉、馬鈴薯澱粉等の根茎澱粉が挙げられる。水溶性セルロース誘導体、及びその塩としては、例えば、カルボキシメチルセルロース、カルボキシメチルセルロースナトリウム等が挙げられる。 The water-soluble polysaccharide component (B) of the present invention is not particularly limited as long as it is a water-soluble polysaccharide commonly used in cosmetics. Specific examples include starch, water-soluble cellulose derivatives, and salts thereof. Examples of starches include seed starches such as rice starch, wheat starch, and corn starch, and rhizome starches such as tapioca starch and potato starch. Examples of water-soluble cellulose derivatives and salts thereof include carboxymethylcellulose and sodium carboxymethylcellulose.

本願発明の構成成分(B)として、好ましくは澱粉である。より好ましくは種実澱粉であり、最も好ましくは米澱粉である。種実澱粉は、根茎澱粉と比較して水膨潤性が低いため、水溶液粘度が比較的低く、ハンドリング性が良い。 The component (B) of the present invention is preferably starch. More preferred is seed starch, and most preferred is rice starch. Seed starch has a lower water swelling property than rhizome starch, and thus has a relatively low aqueous solution viscosity and good handling properties.

本願発明の化粧料用球状複合粉体の複合化工程における、構成成分の水分散体濃度(構成成分(A)と構成成分(B)の含有量を合計した水中濃度)は2~40重量%である。より好ましくは5~20重量%である。40重量%よりも大きいと、構成成分(A)と構成成分(B)を含有する水分散体の粘度が高くなり、ハンドリング性が低下する。2重量%よりも小さいと、固形分濃度が少なくなることで、化粧料用球状複合粉体の収率が低下する。 In the compounding step of the spherical composite powder for cosmetics of the present invention, the concentration of the aqueous dispersion of the constituent components (concentration in water that is the sum of the contents of the constituent component (A) and the constituent component (B)) is 2 to 40% by weight. It is. More preferably, it is 5 to 20% by weight. If it is more than 40% by weight, the viscosity of the aqueous dispersion containing component (A) and component (B) will increase, and the handling properties will decrease. When it is less than 2% by weight, the yield of the spherical composite powder for cosmetics decreases because the solid content concentration decreases.

本願発明で得られる化粧料用球状複合粉体のメディアン径は、3~30μmである。より好ましくは5~20μmである。30μmよりも大きいと粒感を生じ、柔らかい感触特性に劣る。 The median diameter of the spherical composite powder for cosmetics obtained by the present invention is 3 to 30 μm. More preferably, it is 5 to 20 μm. If it is larger than 30 μm, a grainy feel will occur and the soft touch characteristics will be poor.

本願発明で得られる化粧料用球状複合粉体の固形分重量比(鉱物の含有量:水溶性多糖類の含有量)は、98:2~80:20である。より好ましくは95:5~85:15である。水溶性多糖類の構成割合が20重量%よりも大きいと、複合化工程における水分散体の粘度が高くなり、ハンドリング性が低下する。一方、2重量%よりも小さいと、鉱物間のつなぎ成分が少なくなることで、化粧料用球状複合粉体の収率が低下する。 The solid content weight ratio (mineral content:water-soluble polysaccharide content) of the spherical composite powder for cosmetics obtained by the present invention is 98:2 to 80:20. More preferably, the ratio is 95:5 to 85:15. If the proportion of the water-soluble polysaccharide is greater than 20% by weight, the viscosity of the water dispersion in the compositing step will increase, resulting in poor handling. On the other hand, if it is less than 2% by weight, the binding component between minerals will decrease, resulting in a decrease in the yield of spherical composite powder for cosmetics.

本願発明で得られる化粧料用球状複合粉体は、未処理で使用することもできるが、適宜、表面処理を施して使用しても良い。表面処理剤としては、通常、化粧料用粉体に用いられる表面処理剤であれば特に限定されない。具体的な表面処理剤として、例えば、フッ素化合物、シリコーン化合物、エステル化合物、金属石鹸、ロウ、油脂、炭化水素等が挙げられる。 The spherical composite powder for cosmetics obtained by the present invention can be used untreated, but it may also be used after being subjected to surface treatment as appropriate. The surface treatment agent is not particularly limited as long as it is a surface treatment agent that is normally used for powders for cosmetics. Specific examples of surface treatment agents include fluorine compounds, silicone compounds, ester compounds, metal soaps, waxes, oils and fats, hydrocarbons, and the like.

本願発明で得られる化粧料用球状複合粉体は、以下に示す水分散体調製工程(1)、(2)、及び複合化工程(3)を経て調製される。
(1)機械式撹拌機を用いて、水溶性多糖類の水溶液を得る。この際、水溶性多糖類を水中へ溶解させるために、適宜加熱して溶解させることができる。
(2)工程(1)で得られた水溶性多糖類の水溶液に鉱物を添加し、機械式撹拌機を用いて、水分散体を得る。
(3)工程(2)で得られた分散体を噴霧乾燥機に供し、高温場における微細液滴の急速固化により、鉱物と水溶性多糖類からなる化粧料用球状複合粉体を得る。
The spherical composite powder for cosmetics obtained by the present invention is prepared through the following aqueous dispersion preparation steps (1), (2), and composite step (3).
(1) Obtain an aqueous solution of water-soluble polysaccharide using a mechanical stirrer. At this time, in order to dissolve the water-soluble polysaccharide in water, it can be heated and dissolved as appropriate.
(2) A mineral is added to the aqueous solution of the water-soluble polysaccharide obtained in step (1), and an aqueous dispersion is obtained using a mechanical stirrer.
(3) The dispersion obtained in step (2) is subjected to a spray dryer, and the fine droplets are rapidly solidified in a high temperature field to obtain a spherical composite powder for cosmetics consisting of a mineral and a water-soluble polysaccharide.

本願発明の化粧料用球状複合粉体の製造工程(1)、及び(2)において使用される機械式撹拌機は、通常、液中分散操作に用いられる撹拌機であれば特に限定されない。例えば、ディスパーミキサー、ホモミキサー、高圧ホモジナイザー等が挙げられる。 The mechanical stirrer used in the manufacturing steps (1) and (2) of the spherical composite powder for cosmetics of the present invention is not particularly limited as long as it is a stirrer that is normally used for dispersion in liquid. Examples include a disper mixer, a homomixer, a high-pressure homogenizer, and the like.

本願発明の化粧料用球状複合粉体の製造工程(2)において、硫酸アルミニウム(硫酸バンド)やポリ塩化アルミニウム(PAC)等の凝集剤や、その他、無機塩等を用いて水分散体の粘度を適宜調整しても良い。 In the manufacturing process (2) of the spherical composite powder for cosmetics of the present invention, flocculants such as aluminum sulfate (sulfate band) and polyaluminum chloride (PAC), and other inorganic salts are used to reduce the viscosity of the aqueous dispersion. may be adjusted as appropriate.

本願発明の化粧料用球状複合粉体の製造工程(3)において使用される噴霧乾燥機は、通常、造粒体製造に用いられる噴霧乾燥機であれば特に限定されない。噴霧乾燥機は、噴霧機構の違いにより、大きくノズル方式と回転ディスク方式に分類できるが、いずれの噴霧機構を備える噴霧乾燥機も用いることができる。 The spray dryer used in the manufacturing step (3) of the spherical composite powder for cosmetics of the present invention is not particularly limited as long as it is a spray dryer that is normally used for manufacturing granules. Spray dryers can be broadly classified into nozzle type and rotating disk type depending on the difference in spray mechanism, but spray dryers with either type of spray mechanism can be used.

本願発明において、好ましいメディアン径を有する化粧料用球状複合粉体を得るためには、上記噴霧乾燥機のなかでも、特に2流体以上のノズル方式、又は回転ディスク方式噴霧機構を備える噴霧乾燥機を用いることが好ましい。 In the present invention, in order to obtain a spherical composite powder for cosmetics having a preferable median diameter, among the above-mentioned spray dryers, a spray dryer equipped with a two or more fluid nozzle type or a rotating disk type spray mechanism is particularly used. It is preferable to use

以下、実施例により本願発明をさらに詳細に説明する。尚、これらは本願発明を何ら限定するものではない。 Hereinafter, the present invention will be explained in more detail with reference to Examples. Note that these do not limit the present invention in any way.

(製造方法)実施例1~8、比較例1
工程(1):下記表1の成分8~10(水溶性多糖類)を成分11(蒸留水)中に添加し、ホモミキサー(T.K.ロボミックス;プライミクス社製)を用いて水溶液を調製した。成分8、及び9の溶解には、予め90℃に加温した蒸留水を用いた。
工程(2):下記表1の成分1~7(鉱物)を、工程(1)で得た水溶性多糖類の水溶液中に添加し、ホモミキサーを用いて、下記条件により鉱物と水溶性多糖類の水分散体を調製した。この際、水分散体濃度が9.2重量%、及び鉱物と水溶性多糖類の固形分重量比が87:13となるようにそれぞれ調整した。
ホモミキサー回転速度:5000rpm
分散処理時間:30分
工程(3):工程(2)で得られた水分散体を、下記条件のもと噴霧乾燥機(L-12型;大川原化工機社製)に供し、成分1~10からなる化粧料用球状複合粉体を得た。
噴霧方式:回転ディスク
ディスク回転速度:25,000rpm
水分散体流量:160mL/分
給気温度:220℃
排気温度:105℃
(Manufacturing method) Examples 1 to 8, Comparative example 1
Step (1): Components 8 to 10 (water-soluble polysaccharides) in Table 1 below were added to component 11 (distilled water), and the aqueous solution was mixed using a homomixer (T.K. Robomix; manufactured by Primix). Prepared. Distilled water preheated to 90°C was used to dissolve components 8 and 9.
Step (2): Components 1 to 7 (minerals) in Table 1 below are added to the aqueous solution of water-soluble polysaccharide obtained in step (1), and the minerals and water-soluble polysaccharide are mixed using a homomixer under the following conditions. An aqueous dispersion of sugars was prepared. At this time, the concentration of the water dispersion was adjusted to 9.2% by weight, and the solid weight ratio of the mineral to the water-soluble polysaccharide was adjusted to 87:13.
Homo mixer rotation speed: 5000 rpm
Dispersion treatment time: 30 minutes Step (3): The aqueous dispersion obtained in Step (2) was subjected to a spray dryer (Model L-12; manufactured by Okawara Kakoki Co., Ltd.) under the following conditions, and the components 1 to 1 were A spherical composite powder for cosmetics consisting of 10 was obtained.
Spraying method: rotating disc Disc rotation speed: 25,000 rpm
Water dispersion flow rate: 160mL/min Supply air temperature: 220℃
Exhaust temperature: 105℃

(球形性評価方法)
上記実施例、及び比較例の化粧料用球状複合粉体の球形性について、走査型電子顕微鏡を用いて拡大倍率500倍で観察するときに、その観察視野に当該複合粉体が100個以上存在する条件で、円形度が0.95以上の複合粉体を球形とみなし、その個数割合を、以下に示す判定基準に従って判定した。(円形度の計算は、画像解析から複合粉体の投影面積と周長を求め算出した。)
<判定基準>
〔球形と認められる複合粉体の個数割合〕 〔判定〕
75%以上 ◎
50%以上 ○
50%未満 △
25%未満 ×
(Sphericity evaluation method)
Regarding the sphericity of the spherical composite powders for cosmetics of the above examples and comparative examples, when observing the spherical composite powders for cosmetics using a scanning electron microscope at a magnification of 500 times, 100 or more of the composite powders are present in the observation field. Under these conditions, composite powders with a circularity of 0.95 or more were considered to be spherical, and their number ratio was determined according to the criteria shown below. (Circularity was calculated by determining the projected area and circumference of the composite powder from image analysis.)
<Judgment criteria>
[Percentage of number of composite powders recognized as spherical] [Judgment]
75% or more ◎
50% or more ○
Less than 50% △
Less than 25% ×

(柔らかさ評価方法)
20~40代の化粧品専門パネル5名に、上記実施例、及び比較例の化粧料用球状複合粉体を指先、あるいは手の甲に伸ばして柔らかさについて、以下の評価基準により評点を付し、化粧料用球状複合粉体ごとに評点の平均点を算出して、以下に示す判定基準に従って判定した。
<評価基準>
〔使用性〕 〔評点〕
非常に良好 :5
良好 :4
普通 :3
やや不良 :2
不良 :1
<判定基準>
〔評点の平均点〕 〔判定〕
4.5以上 ◎
3.5以上4.5未満 ○
2以上3.5未満 △
2未満 ×
(Softness evaluation method)
A panel of five cosmetics experts in their 20s to 40s spread the spherical composite powders for cosmetics of the above Examples and Comparative Examples on their fingertips or the back of their hands and gave them a score based on the following evaluation criteria. The average score was calculated for each spherical composite powder, and the evaluation was made according to the criteria shown below.
<Evaluation criteria>
[Usability] [Rating]
Very good: 5
Good: 4
Normal: 3
Slightly poor: 2
Defective: 1
<Judgment criteria>
[Average score] [Judgment]
4.5 or more ◎
3.5 or more and less than 4.5 ○
2 or more but less than 3.5 △
Less than 2 ×

※1 ナノエース D-1000F(日本タルク社製)
※2 ナノエース D-600(日本タルク社製)
※3 FG-15F(日本タルク社製)
※4 SG-95(日本タルク社製)
※5 P-3(日本タルク社製)
※6 セリサイト FSE(三信鉱工社製)を、機械的粉砕工程により微粒化
※7 ASP-170(BASF社製)を、機械的粉砕工程により微粒化
*1 Nano Ace D-1000F (manufactured by Nippon Talc Co., Ltd.)
*2 Nano Ace D-600 (manufactured by Nippon Talc Co., Ltd.)
*3 FG-15F (manufactured by Nippon Talc Co., Ltd.)
*4 SG-95 (manufactured by Nippon Talc Co., Ltd.)
*5 P-3 (manufactured by Nippon Talc Co., Ltd.)
*6 Sericite FSE (manufactured by Sanshin Koko Co., Ltd.) is atomized through a mechanical crushing process *7 ASP-170 (manufactured by BASF) is atomized through a mechanical crushing process

表1の実施例1~3で用いた各鉱物(タルク、セリサイト、カオリン)の、40重量%水分散体におけるせん断粘度(せん断速度10/sec)は、それぞれ、81,650、340、2,920mPa・sである。 The shear viscosities (shear rate 10/sec) of each mineral (talc, sericite, kaolin) used in Examples 1 to 3 in Table 1 in a 40% by weight aqueous dispersion were 81,650, 340, and 2, respectively. , 920 mPa·s.

図1に、実施例1で得られた化粧料用球状複合粉体の電子顕微鏡像を示す。非常に球形性の高い球状複合粉体が得られた。 FIG. 1 shows an electron microscope image of the spherical composite powder for cosmetics obtained in Example 1. A spherical composite powder with extremely high sphericity was obtained.

同等のメディアン径を有する鉱物の種類を変えて化粧料用球状複合粉体の製造を実施した結果、いずれも良好な球状複合粉体が得られ、特に鉱物としてタルクを用いた系で最も良好な球形性を有する球状複合粉体が得られた(実施例1~3)。 As a result of producing spherical composite powders for cosmetics by changing the types of minerals with the same median diameter, good spherical composite powders were obtained in all cases, and in particular, the system using talc as the mineral had the best results. Spherical composite powders having sphericity were obtained (Examples 1 to 3).

メディアン径の異なるタルクを用いて化粧料用球状複合粉体の製造を実施した結果、メディアン径2.1μm以下のタルクを用いた系では、良好な球形性を有する球状複合粉体が得られたが、メディアン径5μmのタルクを用いた系では球形性が低下した(実施例1、6~8、比較例1)。 As a result of manufacturing spherical composite powder for cosmetics using talc with different median diameters, it was found that spherical composite powder with good sphericity was obtained in the system using talc with a median diameter of 2.1 μm or less. However, in the system using talc with a median diameter of 5 μm, the sphericity decreased (Examples 1, 6 to 8, Comparative Example 1).

水溶性多糖類の種類を変えて化粧料用球状複合粉体の製造を実施した結果、いずれも良好な球状複合粉体が得られ、特に水溶性多糖類として米澱粉、カルボキシメチルセルロースNaを用いた系で最も良好な球形性を有する球状複合粉体が得られた(実施例1、4、5)。 As a result of producing spherical composite powders for cosmetics by changing the types of water-soluble polysaccharides, good spherical composite powders were obtained in all cases, especially when rice starch and carboxymethyl cellulose Na were used as water-soluble polysaccharides. Spherical composite powders having the best sphericity among the systems were obtained (Examples 1, 4, and 5).

(製造方法)実施例9~14
工程(1):下記表2の成分2を予め90℃に加温した成分3中に添加し、ホモミキサー(T.K.ロボミックス;プライミクス社製)を用いて水溶液を調製した。
工程(2):下記表2の成分1を、工程(1)で得た成分2の水溶液中に添加し、ホモミキサーを用いて、下記条件により鉱物と水溶性多糖類の水分散体を調製した。この際、水分散体濃度が1~45重量%となるように、それぞれ調整した。また、鉱物と水溶性多糖類の固形分重量比が87:13となるように調整した。
ホモミキサー回転速度:5000rpm
分散処理時間:30分
工程(3):工程(2)で得られた水分散体を噴霧乾燥機(MDL-050B型;藤崎電機社製)に供し、成分1、及び2からなる化粧料用球状複合粉体を得た。
噴霧方式:3流体ノズルPN3005
水分散体流量:45mL/分
給気温度:250℃
排気温度:105℃
(Manufacturing method) Examples 9 to 14
Step (1): Component 2 in Table 2 below was added to Component 3 that had been previously heated to 90° C., and an aqueous solution was prepared using a homomixer (T.K. Robomix; manufactured by Primix Co., Ltd.).
Step (2): Add component 1 in Table 2 below to the aqueous solution of component 2 obtained in step (1), and use a homomixer to prepare an aqueous dispersion of minerals and water-soluble polysaccharides under the following conditions. did. At this time, the concentration of the water dispersion was adjusted to be 1 to 45% by weight. Further, the solid content weight ratio of mineral and water-soluble polysaccharide was adjusted to be 87:13.
Homo mixer rotation speed: 5000 rpm
Dispersion treatment time: 30 minutes Step (3): The aqueous dispersion obtained in Step (2) is subjected to a spray dryer (model MDL-050B; manufactured by Fujisaki Electric Co., Ltd.) to obtain a cosmetic composition consisting of components 1 and 2. A spherical composite powder was obtained.
Spraying method: 3 fluid nozzle PN3005
Water dispersion flow rate: 45mL/min Supply air temperature: 250℃
Exhaust temperature: 105℃

表2の実施例9~14では、タルクと米澱粉の固形分重量比を87:13に固定し、水分散体濃度を変えて化粧料用球状複合粉体の製造を実施した。構成成分の水分散体濃度が2~40重量%の系では、良好な球形性、及び柔らかさを有する球状複合粉体が得られ、特に構成成分の水分散体濃度が5重量%、及び20重量%の系で、最も良好な球形性、及び柔らかさを有する球状複合粉体が得られた(実施例9~12)。構成成分の水分散体濃度が1重量%の系では、実施例9~12と比較して球状複合粉体の収率が低く、球形性、及び柔らかさも劣る結果であった(実施例13)。また構成成分の水分散体濃度が45重量%の系では、球状複合粉体の収率は高かったが、実施例9~12と比較して球形性、及び柔らかさで劣る結果であった(実施例14)。 In Examples 9 to 14 shown in Table 2, spherical composite powders for cosmetics were produced by fixing the solid content weight ratio of talc and rice starch at 87:13 and varying the water dispersion concentration. In systems where the aqueous dispersion concentration of the constituent components is 2 to 40% by weight, a spherical composite powder with good sphericity and softness can be obtained. % by weight, spherical composite powders having the best sphericity and softness were obtained (Examples 9 to 12). In a system where the water dispersion concentration of the constituent components was 1% by weight, the yield of spherical composite powder was lower than in Examples 9 to 12, and the sphericity and softness were also inferior (Example 13). . In addition, in a system where the concentration of the aqueous dispersion of the constituent components was 45% by weight, the yield of spherical composite powder was high, but the results were inferior in sphericity and softness compared to Examples 9 to 12. Example 14).

(製造方法)実施例15~20
工程(1):下記表3の成分2を予め90℃に加温した成分3中に添加し、ホモミキサー(T.K.ロボミックス;プライミクス社製)を用いて水溶液を調製した。
工程(2):下記表3の成分1を、工程(1)で得た成分2の水溶液中に添加し、ホモミキサーを用いて、下記条件により鉱物と水溶性多糖類の水分散体を調製した。この際、鉱物と水溶性多糖類の固形分重量比が1:99~75:25となるように、それぞれ調整した。また、水分散体濃度が9.2重量%となるように調整した。
ホモミキサー回転速度:5000rpm
分散処理時間:30分
工程(3):工程(2)で得られた水分散体を噴霧乾燥機(MDL-050B型;藤崎電機社製)に供し、成分1、及び2からなる化粧料用球状複合粉体を得た。
噴霧方式:4流体ノズルSE4003
水分散体流量:45mL/分
給気温度:250℃
排気温度:105℃
(Production method) Examples 15 to 20
Step (1): Component 2 in Table 3 below was added to Component 3 that had been previously heated to 90° C., and an aqueous solution was prepared using a homomixer (T.K. Robomix; manufactured by Primix).
Step (2): Add component 1 in Table 3 below to the aqueous solution of component 2 obtained in step (1), and use a homomixer to prepare an aqueous dispersion of minerals and water-soluble polysaccharides under the following conditions. did. At this time, the solid content weight ratio of mineral and water-soluble polysaccharide was adjusted to be 1:99 to 75:25. Further, the concentration of the water dispersion was adjusted to 9.2% by weight.
Homo mixer rotation speed: 5000 rpm
Dispersion treatment time: 30 minutes Step (3): The aqueous dispersion obtained in Step (2) is subjected to a spray dryer (model MDL-050B; manufactured by Fujisaki Electric Co., Ltd.) to obtain a cosmetic composition consisting of components 1 and 2. A spherical composite powder was obtained.
Spraying method: 4 fluid nozzle SE4003
Water dispersion flow rate: 45mL/min Supply air temperature: 250℃
Exhaust temperature: 105℃

表3の実施例15~20では、タルクと米澱粉の水分散体濃度を9.2重量%に固定し、固形分重量比を変えて化粧料用球状複合粉体の製造を実施した。構成成分の固形分重量比が98:2~80:20の系では、良好な球形性、及び柔らかさを有する球状複合粉体が得られ、特に構成成分の固形分重量比が95:5、及び85:15の系で、最も良好な球形性、及び柔らかさを有する球状複合粉体が得られた(実施例15~18)。構成成分の固形分重量比が99:1、及び75:25の系では、実施例15~18と比較して、いずれも球状複合粉体の球形性、及び柔らかさで劣る結果であった(実施例19、20)。 In Examples 15 to 20 of Table 3, spherical composite powders for cosmetics were produced by fixing the concentration of the aqueous dispersion of talc and rice starch at 9.2% by weight and varying the solid content weight ratio. In a system where the solid content weight ratio of the constituent components is 98:2 to 80:20, a spherical composite powder having good sphericity and softness can be obtained, and especially when the solid content weight ratio of the constituent components is 95:5, and 85:15, spherical composite powders with the best sphericity and softness were obtained (Examples 15 to 18). In systems where the solid content weight ratio of the constituent components was 99:1 and 75:25, the results were that the spherical composite powders were inferior in sphericity and softness compared to Examples 15 to 18 ( Examples 19, 20).

本願発明は、柔らかい感触を有する従来の合成ポリマーに代替しうる感触特性を有する環境適合性の化粧料用球状複合粉体、及びその製造方法を提供するものである。本願発明の化粧料用球状複合粉体を用いれば、環境に配慮した化粧品製剤を開発することができる。
The present invention provides an environmentally compatible spherical composite powder for cosmetics that has tactile properties that can replace conventional synthetic polymers that have a soft feel, and a method for producing the same. By using the spherical composite powder for cosmetics of the present invention, it is possible to develop environmentally friendly cosmetic formulations.

Claims (5)

構成成分として、下記成分(A)、及び(B)を含有する化粧料用球状複合粉体。
(A)メディアン径が0.5~2.1μmのタルクであり、その40重量%水分散体をE型粘度計で測定したときのせん断粘度(せん断速度10/sec)が10,000mPa・s以上となる物理特性を有するもの
(B)孔を有さない水溶性多糖類
A spherical composite powder for cosmetics containing the following components (A) and (B) as constituent components.
(A) Talc with a median diameter of 0.5 to 2.1 μm, and a shear viscosity (shear rate of 10/sec) of 40% by weight water dispersion measured with an E-type viscometer of 10,000 mPa・s Items with the above physical properties
(B) Water-soluble polysaccharide without pores
構成成分(B)が、孔を有さない澱粉であることを特徴とする請求項1記載の化粧料用球状複合粉体。 The spherical composite powder for cosmetics according to claim 1, wherein the component (B) is starch without pores. 構成成分(B)が、孔を有さない種実澱粉であることを特徴とする請求項1又は2記載の化粧料用球状複合粉体。 The spherical composite powder for cosmetics according to claim 1 or 2, wherein the component (B) is seed starch without pores. 構成成分(A)と構成成分(B)の重量比が、98:2~80:20であることを特徴とする請求項1~3のいずれか一項記載の化粧料用球状複合粉体。 The spherical composite powder for cosmetics according to any one of claims 1 to 3, wherein the weight ratio of component (A) to component (B) is 98:2 to 80:20. 下記工程(1)~(3)を経て調製される、請求項1~4のいずれか一項記載の化粧料用球状複合粉体の製造方法。
工程(1):機械式撹拌機を用いて、水溶性多糖類の水溶液を得る。
工程(2):工程(1)で得られた水溶性多糖類の水溶液に鉱物を添加し、機械式撹拌機を用いて、水分散体を得る。
工程(3):工程(2)で得られた分散体を噴霧乾燥機に供し、高温場における微細液滴の急速固化により、鉱物と水溶性多糖類からなる化粧料用球状複合粉体を得る。

A method for producing a spherical composite powder for cosmetics according to any one of claims 1 to 4, which is prepared through the following steps (1) to (3).
Step (1): Using a mechanical stirrer, an aqueous solution of water-soluble polysaccharide is obtained.
Step (2): A mineral is added to the aqueous solution of the water-soluble polysaccharide obtained in step (1), and an aqueous dispersion is obtained using a mechanical stirrer.
Step (3): The dispersion obtained in step (2) is subjected to a spray dryer, and the fine droplets are rapidly solidified in a high temperature field to obtain a spherical composite powder for cosmetics consisting of minerals and water-soluble polysaccharides. .

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JPS6366111A (en) * 1986-09-05 1988-03-24 Shiseido Co Ltd Cosmetic blended with spherical organic complex clay mineral
DE3750576T2 (en) * 1986-07-24 1995-04-27 Shiseido Co Ltd SPHERICAL SMALL POWDER, METHOD FOR THE PRODUCTION AND COMPOSITION THAT CONTAINS THIS.
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