JP6482944B2 - Polylactic acid short fibers and makeup cosmetics containing the same - Google Patents
Polylactic acid short fibers and makeup cosmetics containing the same Download PDFInfo
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- JP6482944B2 JP6482944B2 JP2015094132A JP2015094132A JP6482944B2 JP 6482944 B2 JP6482944 B2 JP 6482944B2 JP 2015094132 A JP2015094132 A JP 2015094132A JP 2015094132 A JP2015094132 A JP 2015094132A JP 6482944 B2 JP6482944 B2 JP 6482944B2
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- 239000000835 fiber Substances 0.000 title claims description 195
- 229920000747 poly(lactic acid) Polymers 0.000 title claims description 94
- 239000004626 polylactic acid Substances 0.000 title claims description 94
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- 229910052785 arsenic Inorganic materials 0.000 claims description 11
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- 238000000034 method Methods 0.000 description 24
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- 239000003086 colorant Substances 0.000 description 4
- LHRCREOYAASXPZ-UHFFFAOYSA-N dibenz[a,h]anthracene Chemical compound C1=CC=C2C(C=C3C=CC=4C(C3=C3)=CC=CC=4)=C3C=CC2=C1 LHRCREOYAASXPZ-UHFFFAOYSA-N 0.000 description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
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- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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- 238000010000 carbonizing Methods 0.000 description 1
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- 238000004898 kneading Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000006233 lamp black Substances 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
- 229960003493 octyltriethoxysilane Drugs 0.000 description 1
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Cosmetics (AREA)
- Artificial Filaments (AREA)
Description
本発明は、ポリ乳酸短繊維と、そのポリ乳酸短繊維を含有するメークアップ化粧料に関するものである。 The present invention relates to a polylactic acid short fiber and a makeup cosmetic containing the polylactic acid short fiber.
従来から、短繊維を化粧料に配合することは、特許文献１のように、アイメークアップ化粧料において、睫毛や眉毛にボリューム感を付与したり、特許文献２のように、疑似的な肌理構造を肌上に構築したりする目的で、ファンデーションなどのメークアップ化粧料等で試みられている。更に、特許文献３，４などには、繊維の断面形状等に特徴をもたせることで、マスカラに配合した際、様々な光学効果や付着親和性の改良がなされている。このように短繊維は、メークアップ化粧料に多く用いられている。近年では、形状だけでなく、特許文献５に示すような、剛直な繊維を配合することも行われている。 Conventionally, blending short fibers into cosmetics, like Patent Document 1, in eye makeup cosmetics, gives a voluminous feel to the eyelashes and eyebrows, or has a pseudo-texture structure as in Patent Document 2. Has been tried with makeup cosmetics such as foundations for the purpose of constructing skin on the skin. Furthermore, Patent Documents 3 and 4 and the like have various optical effects and improved adhesion affinity when blended into a mascara by giving a characteristic to the cross-sectional shape of the fiber. As described above, short fibers are often used in makeup cosmetics. In recent years, not only the shape but also a rigid fiber as shown in Patent Document 5 has been blended.
一方、ポリ乳酸などの生分解性ポリマーは、化粧料として使用された後に自然界に放出されても容易に分解するため、環境への負荷が小さく注目されており、例えば特許文献６のようにポリ乳酸粉体を化粧品に配合することが提案されている。 On the other hand, biodegradable polymers such as polylactic acid are easily decomposed even when released into nature after being used as cosmetics. It has been proposed to blend lactic acid powder into cosmetics.
ところで、特許文献１〜５に係る短繊維では、自然界中で容易に分解しないものがあり、化粧料として使用された後に自然界に放出されると、長時間ゴミや堆積物として存在するなど環境への負荷が大きいという問題点がある。
そこで、特許文献６に係るポリ乳酸粉体を用いることが考えられるが、粉体状であるため、粉体相互の繋がりが弱く、例えばアイメークアップ化粧料において睫毛や眉毛にボリューム感を与えることができず、また疑似的な肌理構造を肌上に構築することができないという問題点がある。
By the way, some short fibers according to Patent Documents 1 to 5 are not easily decomposed in the natural world, and when released into the natural world after being used as a cosmetic, they exist as dust or deposits for a long time. There is a problem that the load of is large.
Then, although it is possible to use the polylactic acid powder which concerns on patent document 6, since it is a powder form, the connection between powder is weak, for example, it may give a volume feeling to eyelashes and eyebrows in eye makeup cosmetics. In addition, there is a problem that a pseudo-texture structure cannot be constructed on the skin.
本発明は、前述のような問題点に鑑みてなされたもので、環境への負荷が小さく、メークアップ化粧料において、睫毛や眉毛にボリューム感を付与することができるとともに、肌の肌理を再現することができるポリ乳酸短繊維を提供し、併せて、このポリ乳酸短繊維を含有することにより、美しい仕上がりが得られるメークアップ化粧料を提供することを目的とするものである。さらに、ポリ乳酸短繊維の形状維持機能を利用することにより、化粧料使用後は直線状の形状になりながら、マスカラブラシなど化粧料塗布具には変形してより多くの繊維が付着できることを利用して、睫毛や眉毛にボリューム感を付与する効果がより高く得られるメークアップ化粧料を提供することを目的とするものである。 The present invention has been made in view of the above-described problems, has a low environmental load, and can provide volume to eyelashes and eyebrows in makeup cosmetics, and reproduces the texture of the skin. It is an object of the present invention to provide a make-up cosmetic that can provide a beautiful finish by providing a short polylactic acid fiber that can be produced, and also containing the short polylactic acid fiber. In addition, by utilizing the shape maintenance function of polylactic acid short fibers, it is possible to deform a cosmetic applicator such as a mascara brush and attach more fibers while it is in a linear shape after cosmetic use. Then, it aims at providing the makeup cosmetics from which the effect which gives a volume feeling to eyelashes and eyebrows is obtained more highly.
本発明者らは鋭意研究を重ねた結果、生分解性ポリマーであるポリ乳酸を用いて短繊維を調製し、該短繊維をメークアップ化粧料に配合することにより、メークアップ化粧料において、睫毛や眉毛にボリューム感を付与することができるとともに、肌の肌理を再現することができ、更に該短繊維を特定の要件を満足するカーボンブラック、黒酸化鉄又は炭微粒粉で着色した短繊維をメークアップ化粧料に配合することにより、睫毛や眉毛にボリューム感をより効果的に付与することができるなどの美しい仕上がりが得られることを見出し、本発明を完成させるに至ったものである。さらに、ポリ乳酸短繊維の形状維持機能を利用することにより、化粧料使用後は直線状の形状になり化粧効果を高めながら、マスカラブラシなど化粧料塗布具には変形してより多くの繊維が付着できるため、睫毛や眉毛にボリューム感を付与する効果がより高く得られることも見出している。 As a result of extensive research, the present inventors have prepared short fibers using polylactic acid, which is a biodegradable polymer, and blended the short fibers into the makeup cosmetics. A short fiber colored with carbon black, black iron oxide or charcoal fine powder that can give a sense of volume to the eyebrows and can reproduce the texture of the skin, and further satisfies the specific requirements. It has been found that by adding it to a makeup cosmetic, it is possible to obtain a beautiful finish such as a more effective volume to eyelashes and eyebrows, and the present invention has been completed. Furthermore, by using the shape maintenance function of polylactic acid short fibers, the cosmetic applicator, such as a mascara brush, is deformed and has more fibers while improving the cosmetic effect after using cosmetics. Since it can adhere, it has also been found that the effect of imparting a volume feeling to the eyelashes and eyebrows can be obtained higher.
要するに、前記目的を達成するために、第１発明によるポリ乳酸短繊維は、
繊維長が０．１〜１０．０ｍｍで、繊維径が０．５〜２０デニールであることを特徴とするものである。
In short, in order to achieve the object, the polylactic acid short fiber according to the first invention is:
The fiber length is 0.1 to 10.0 mm, and the fiber diameter is 0.5 to 20 denier.
第１発明において、以下の要件（１）〜（３）を満足するカーボンブラックを繊維の質量に対して０．１〜１０．０質量％配合することを特徴とするものである（第２発明）。
要件（１）：ファーネス法で製造されたものであること
要件（２）：比表面積が４０〜２６０ｍ２／ｇの範囲であること
要件（３）：砒素含有量が３ｐｐｍ以下であること
In the first invention, carbon black satisfying the following requirements (1) to (3) is blended in an amount of 0.1 to 10.0% by mass with respect to the mass of the fiber (second invention) ).
Requirement (1): manufactured by the furnace method Requirement (2): Specific surface area is in the range of 40 to 260 m 2 / g Requirement (3): Arsenic content is 3 ppm or less
第１発明において、以下の要件（１）〜（３）を満足する黒酸化鉄を繊維の質量に対して０．１〜２０．０質量％配合することを特徴とするものである（第３発明）。
要件（１）：中位径が０．１〜５μｍの範囲であること
要件（２）：砒素含有量が３ｐｐｍ以下であること
要件（３）：重金属含有量が３０ｐｐｍ以下であること
In the first invention, black iron oxide satisfying the following requirements (1) to (3) is blended in an amount of 0.1 to 20.0% by mass with respect to the mass of the fiber (third) invention).
Requirement (1): Median diameter is in the range of 0.1 to 5 μm Requirement (2): Arsenic content is 3 ppm or less Requirement (3): Heavy metal content is 30 ppm or less
第１発明において、以下の要件（１）〜（３）を満足する炭微粒粉を繊維の質量に対して０．１〜２０．０質量％配合することを特徴とするものである（第４発明）。
要件（１）：植物由来炭を微粉砕した微粒粉であること
要件（２）：中位径が０．１〜１０μｍの範囲であること
要件（３）：砒素含有量が２ｐｐｍ以下であること
1st invention WHEREIN: 0.1-20.0 mass% is mix | blended with the carbon fine particle powder which satisfies the following requirements (1)-(3) with respect to the mass of a fiber. invention).
Requirement (1): A fine powder obtained by finely pulverizing plant-derived charcoal Requirement (2): The median diameter is in the range of 0.1 to 10 μm Requirement (3): Arsenic content is 2 ppm or less
次に、第５発明によるメークアップ化粧料は、第１発明、第２発明、第３発明又は第４発明に係るポリ乳酸短繊維を含有してなることを特徴とするものである。 Next, the makeup cosmetic according to the fifth invention is characterized by containing the polylactic acid short fibers according to the first invention, the second invention, the third invention or the fourth invention.
第１発明のポリ乳酸短繊維によれば、繊維長が０．１〜１０．０ｍｍで、繊維径が０．５〜２０デニールとされるので、環境への負荷が小さく、メークアップ化粧料において、睫毛や眉毛にボリューム感を付与することができるとともに、肌の肌理を再現することができる。 According to the polylactic acid short fiber of the first invention, since the fiber length is 0.1 to 10.0 mm and the fiber diameter is 0.5 to 20 denier, the load on the environment is small, and in makeup cosmetics In addition to giving a volume to eyelashes and eyebrows, the texture of the skin can be reproduced.
第２発明〜第４発明のポリ乳酸短繊維によれば、特定の要件を満足するカーボンブラック、黒酸化鉄又は炭微粒粉の黒色着色剤によってポリ乳酸短繊維が黒色に着色されるので、睫毛や眉毛にボリューム感をより効果的に付与することができる。 According to the polylactic acid short fibers of the second invention to the fourth invention, the polylactic acid short fibers are colored black by the black colorant of carbon black, black iron oxide or charcoal fine powder satisfying specific requirements. A volume feeling can be given to eyebrows and eyebrows more effectively.
第５発明によれば、第１発明、第２発明、第３発明又は第４発明のポリ乳酸短繊維を含有することにより、環境への負荷が小さく、睫毛や眉毛にボリューム感を付与でき、肌の肌理を再現できるなどの美しい仕上がりのメークアップ化粧料を得ることができる。 According to the fifth invention, by containing the polylactic acid short fiber of the first invention, the second invention, the third invention or the fourth invention, the load on the environment is small, and a volume feeling can be imparted to the eyelashes and eyebrows, Makeup cosmetics with a beautiful finish that can reproduce the texture of the skin.
次に、本発明によるポリ乳酸短繊維及びそれを含有するメークアップ化粧料の具体的な実施の形態について説明する。 Next, specific embodiments of the polylactic acid short fibers according to the present invention and makeup cosmetics containing the same will be described.
＜ポリ乳酸短繊維の説明＞
本発明のポリ乳酸短繊維を作製するには、先ず、周知の溶融紡糸法あるいは溶液紡糸法、湿式紡糸法などを用いて、ポリ乳酸を繊維化する。このようにして得られる繊維の断面形状は、紡糸時にノズルの形状が、円形、星型、Ｙ型など様々な形状や太さのものから選択することよって制御できる。次に、裁断機を通して目的の長さに切り揃えて短繊維化する。本発明の短繊維は、繊維長が０．１〜１０．０ｍｍの範囲にあり、かつ繊維径が０．５〜２０デニールの範囲にあるものを用いる。これは、メークアップ化粧料に配合した際、使用特性に優れていることから選択された範囲である。
繊維長が０．１ｍｍを下回ると、繊維が短すぎるため、繊維相互間の繋がりが弱くなり、ボリューム感が不足し、１０．０ｍｍを超えると、繊維が長すぎるため、例えばアイメークアップ化粧料において、アプリケータのブラシに絡みついて睫毛や眉毛への乗り移りが悪くなる。
繊維径が０．５デニールを下回ると、繊維が細すぎるため、例えばアイメークアップ化粧料において、アプリケータのブラシに絡み付いて睫毛や眉毛への乗り移りが悪くなり、２０デニールを超えると、繊維が太すぎるため、重くなり、長い睫毛が得られにくく、塗った後、違和感がある。
<Description of polylactic acid staple fiber>
In order to produce the polylactic acid short fiber of the present invention, first, polylactic acid is fiberized using a known melt spinning method, solution spinning method, wet spinning method or the like. The cross-sectional shape of the fiber thus obtained can be controlled by selecting the shape of the nozzle during spinning from various shapes and thicknesses such as a circle, a star, and a Y shape. Next, the fiber is cut into a desired length through a cutting machine to make a short fiber. The short fiber of the present invention uses a fiber having a fiber length in the range of 0.1 to 10.0 mm and a fiber diameter in the range of 0.5 to 20 denier. This is a range selected because it has excellent use characteristics when blended into a makeup cosmetic.
When the fiber length is less than 0.1 mm, the fibers are too short, so the connection between the fibers is weak, and the sense of volume is insufficient. When the fiber length exceeds 10.0 mm, the fibers are too long. For example, in eye makeup cosmetics Entangled with the applicator brush, the transfer to the eyelashes and eyebrows becomes worse.
When the fiber diameter is less than 0.5 denier, the fiber is too thin. For example, in eye makeup cosmetics, the transfer to the eyelashes and eyebrows becomes entangled with the brush of the applicator, and when the fiber diameter exceeds 20 denier, the fiber becomes thicker. It is too heavy and it is difficult to obtain long eyelashes.
＜カーボンブラック配合ポリ乳酸短繊維の説明＞
本発明のカーボンブラック配合ポリ乳酸短繊維は、黒色着色材として以下の要件（１）〜（３）を満足するカーボンブラックを繊維の質量に対して０．１〜１０．０質量％配合することを特徴とする。
要件（１）：ファーネス法で製造されたものであること
要件（２）：比表面積が４０〜２６０ｍ２／ｇの範囲であること
要件（３）：砒素含有量が３ｐｐｍ以下であること
ここで上記の用語の解説および定義について以下に示す。
本発明で用いるカーボンブラックは、ファーネス法（又はオイルファーネス法）で製造されたものを用い、サーマル法、アセチレンブラック法、ランプブラック法、チャンネルブラック法などで製造されたものは用いない。これは、ファーネス法以外の方法で製造されたものは、安全性上に何らかの問題がある場合があり、本カーボンブラック配合ポリ乳酸短繊維は目粘膜付近で使用されることからより高い安全性を考慮したものである。ファーネス法の概略としては、石炭系オイルなどを高温雰囲気中に高圧噴霧し、不完全燃焼雰囲気条件下で熱分解してカーボンブラックを得るものである。本発明で用いるカーボンブラックは比表面積が４０〜２６０ｍ２／ｇの範囲にあるものが用いられ、より好ましくは２００〜２６０ｍ２／ｇの範囲にあるものを用いるが、ここで言う比表面積はＢＥＴ法を用い、吸着ガスとして窒素を用いた場合の値である。比表面積がこの範囲にあると、繊維への練り込み特性と発色の良さが両立し、配合特性に優れるメリットがある。次に砒素の含有量であるが、これは化粧品原料基準（粧原基）の一般試験法又は原子吸光法などの分析方法にて分析した場合に、３ｐｐｍ以下であることが必要である。これにより、より高い安全性が確保できるメリットがある。
<Description of carbon black blended polylactic acid short fiber>
The carbon black-containing polylactic acid short fiber of the present invention contains 0.1 to 10.0% by mass of carbon black that satisfies the following requirements (1) to (3) as a black colorant with respect to the mass of the fiber. It is characterized by.
Requirement (1): manufactured by the furnace method Requirement (2): Specific surface area is in the range of 40 to 260 m 2 / g Requirement (3): Arsenic content is 3 ppm or less The explanation and definition of the above terms are shown below.
The carbon black used in the present invention is one produced by the furnace method (or oil furnace method), and one produced by the thermal method, acetylene black method, lamp black method, channel black method or the like is not used. This is because products manufactured by methods other than the furnace method may have some safety problems, and this carbon black-containing polylactic acid short fiber is used near the mucous membrane of the eye, so it is safer. It is taken into consideration. As an outline of the furnace method, coal-based oil or the like is sprayed at high pressure in a high temperature atmosphere, and is thermally decomposed under incomplete combustion atmosphere conditions to obtain carbon black. The carbon black used in the present invention has a specific surface area in the range of 40 to 260 m 2 / g, and more preferably in the range of 200 to 260 m 2 / g. This is the value when nitrogen is used as the adsorption gas. When the specific surface area is within this range, there are merits that the kneading property to the fiber and the good color development are compatible and the blending property is excellent. Next, the content of arsenic, which is required to be 3 ppm or less when analyzed by an analytical method such as a general test method of cosmetic raw material standards (a cosmetic base) or an atomic absorption method. Thereby, there is an advantage that higher safety can be secured.
本発明で用いるカーボンブラックの要件としては、上記以外のスペックとして、例えば以下のような規格を満たしていることが好ましい。なお、試験方法としては常法を用いることができ、特に規定のあるものを以下に記載する。このような規格のカーボンブラックを使うことで製品の安全性を高め、品質的に安定した製品を得ることができる。
強熱減量 ２質量％以下
灰分 ０．１５％以下
鉛 １０ｐｐｍ以下
水銀 １ｐｐｍ以下
全硫酸分 ０．６５％以下
多環芳香族炭化水素類（ＰＡＨｓ） ０．５ｐｐｍ以下
ベンゾ [ｅ] ピレン ５ｐｐｂ以下
ジベンズ [ａ，ｈ] アントラセン ５ｐｐｂ以下
総炭素量 ９５％以上
なお、強熱減量の試験方法としては、１２５℃にて１時間乾燥した後、９５０℃で７分間乾燥した場合の質量減少を測定したものが挙げられる。多環芳香族炭化水素類（ＰＡＨｓ）、ベンゾ [ｅ] ピレン、ジベンズ [ａ，ｈ] アントラセンの分析は、ガスクロマトグラフィー質量分析機（ＧＣＭＳ）を用いることが好ましい。
As requirements for the carbon black used in the present invention, it is preferable that the following specifications are satisfied as specifications other than those described above. In addition, a conventional method can be used as the test method, and particularly specified ones are described below. By using such a standard of carbon black, it is possible to increase the safety of the product and obtain a product that is stable in quality.
Loss on ignition 2% by mass or less Ash 0.15% or less Lead 10ppm or less Mercury 1ppm or less Total sulfuric acid content 0.65% or less Polycyclic aromatic hydrocarbons (PAHs) 0.5ppm or less Benzo [e] Pyrene 5ppb or less Dibenz [ a, h] Anthracene 5 ppb or less Total carbon content 95% or more In addition, as a test method for loss on ignition, the one measured by mass decrease when dried at 950 ° C. for 7 minutes after being dried at 125 ° C. for 1 hour. Can be mentioned. For analysis of polycyclic aromatic hydrocarbons (PAHs), benzo [e] pyrene, dibenz [a, h] anthracene, it is preferable to use a gas chromatography mass spectrometer (GCMS).
本発明のカーボンブラック配合ポリ乳酸短繊維は、上記の要件を満足するカーボンブラックを繊維の質量に対して０．１〜１０．０質量％、より好ましくは０．１〜２．０質量％の範囲で配合する。カーボンブラックの配合量が０．１質量％未満では、着色力が足りず着色の効果得られず、１０質量％超では紡糸時に糸切れが発生して繊維が得られない。本発明のカーボンブラック配合ポリ乳酸短繊維は、原料としてポリ乳酸に該カーボンブラックをあらかじめ配合混合しておく他はカーボンブラック未配合のポリ乳酸短繊維と同じ製法で調製できる。なお、予備分散に用いられる分散機としては、単軸押出機、二軸押出機、ニーダー、ロール、乾式ボールミル、湿式ボールミル、加圧乳化装置などが挙げられる。 The carbon black blended polylactic acid short fiber of the present invention is 0.1 to 10.0% by mass, more preferably 0.1 to 2.0% by mass of carbon black satisfying the above requirements with respect to the mass of the fiber. Mix in the range. If the blending amount of carbon black is less than 0.1% by mass, the coloring power is insufficient and the effect of coloring cannot be obtained. If it exceeds 10% by mass, yarn breakage occurs during spinning and fibers cannot be obtained. The carbon black-blended polylactic acid short fibers of the present invention can be prepared by the same production method as the carbon black-unblended polylactic acid short fibers, except that the carbon black is previously blended with polylactic acid as a raw material. Examples of the disperser used for the preliminary dispersion include a single screw extruder, a twin screw extruder, a kneader, a roll, a dry ball mill, a wet ball mill, and a pressure emulsifier.
＜黒酸化鉄配合ポリ乳酸短繊維の説明＞
本発明の黒酸化鉄配合ポリ乳酸短繊維は、黒色着色剤として以下の要件（１）〜（３）を満足する黒酸化鉄を繊維の質量に対して０．１〜２０．０質量％配合することを特徴とするものである。
要件（１）：中位径が０．１〜５μｍの範囲であること
要件（２）：砒素含有量が３ｐｐｍ以下であること
要件（３）：重金属含有量が３０ｐｐｍ以下であること
ここで中位径は、黒顔料の発色性と分散性に影響し、粒子径が小さいと分散性が悪くなり、大きいと発色性が悪く黒色度が低くなる。また黒酸化鉄中の砒素、重金属含有量は、粧原基一般試験法又は原子吸光法などで分析でき、眼粘膜付近で使用する場合は、いずれも低い濃度であることが必要である。
<Description of black iron oxide blended polylactic acid staple fiber>
The black iron oxide-containing polylactic acid short fiber of the present invention contains 0.1 to 20.0% by mass of black iron oxide satisfying the following requirements (1) to (3) as a black colorant with respect to the mass of the fiber. It is characterized by doing.
Requirement (1): Median diameter is in the range of 0.1 to 5 μm Requirement (2): Arsenic content is 3 ppm or less Requirement (3): Heavy metal content is 30 ppm or less The unit diameter affects the color developability and dispersibility of the black pigment. When the particle size is small, the dispersibility is poor, and when it is large, the color developability is poor and the blackness is low. The arsenic and heavy metal contents in black iron oxide can be analyzed by a general test method for cosmetic primordium or atomic absorption method, and when used in the vicinity of the ocular mucosa, both must be at low concentrations.
また別に、更に分散性や発色性を高める目的で、該黒酸化鉄に予め下記一般式 [１]で示されるアルキルトリアルコキシシランを用いて表面処理してもよい。表面処理量は、黒酸化鉄に対して０．１〜１０質量％がよく、好ましくは１〜５質量％が適当である。
ＣＨ３−（ＣＨ２）ｎ−Ｓｉ−（ＯＣｍＨ２ｍ＋１）３・・・[１]
（式中、ｎは７〜１４の整数であり、ｍは１又は２の整数である。）
アルキルトリアルコキシシランによる表面処理は、黒酸化鉄表面を疎水性にし、ポリ乳酸中への分散性をさらに向上させることができる。
In addition, for the purpose of further improving dispersibility and color developability, the black iron oxide may be surface-treated with an alkyltrialkoxysilane represented by the following general formula [1] in advance. The surface treatment amount is preferably from 0.1 to 10% by mass, preferably from 1 to 5% by mass, based on black iron oxide.
CH 3 - (CH 2) n -Si- (OC m H 2m + 1) 3 ··· [1]
(In the formula, n is an integer of 7 to 14, and m is an integer of 1 or 2.)
Surface treatment with an alkyltrialkoxysilane can make the black iron oxide surface hydrophobic and further improve dispersibility in polylactic acid.
次に、繊維へ配合する黒酸化鉄の濃度は、短繊維総重量中に０．１〜２０質量％配合される。配合量が０．１質量％よりも少なすぎる場合は、着色力が弱く、発色性が不足し、配合量が２０質量％よりも多すぎる場合は、繊維の柔軟性や紡糸性が劣るものになる。さらに繊維中の顔料粒子分散性は、３００ｍｅｓｈパス相当であり、目開き４５μｍであるので、少なくとも分散粒子径４５μｍ以下であると考えられる。これより大きな分散粒子径を有している場合、繊維紡糸時に糸切れなどを起こし、安定して紡糸することはできない。これは酸化鉄を混色にし、複合着色顔料として使用する場合についても同様である。本発明の黒酸化鉄配合ポリ乳酸短繊維は、ポリ乳酸に該黒酸化鉄をあらかじめ、各種予備分散機にて分散させた配合原料を作製しておく他は黒酸化鉄未配合のポリ乳酸短繊維と同じ製法で調製できる。なお、予備分散に用いられる分散機としては、単軸押出機、二軸押出機、ニーダー、ロール、乾式ボールミル、湿式ボールミル、加圧乳化装置などが挙げられる。 Next, the concentration of black iron oxide to be mixed into the fiber is 0.1 to 20% by mass in the total weight of the short fibers. When the blending amount is less than 0.1% by mass, the coloring power is weak and the color developability is insufficient. When the blending amount is more than 20% by mass, the flexibility and spinnability of the fiber is inferior. Become. Furthermore, the dispersibility of the pigment particles in the fiber is equivalent to a 300 mesh pass and has an opening of 45 μm, so it is considered that the dispersed particle diameter is at least 45 μm or less. When the dispersed particle diameter is larger than this, yarn breakage occurs during fiber spinning, and stable spinning cannot be performed. The same applies to the case where iron oxide is mixed and used as a composite coloring pigment. The black iron oxide-blended polylactic acid short fiber of the present invention is prepared by preparing a blended raw material in which the black iron oxide is previously dispersed in polylactic acid by various pre-dispersing machines. It can be prepared by the same manufacturing method as the fiber. Examples of the disperser used for the preliminary dispersion include a single screw extruder, a twin screw extruder, a kneader, a roll, a dry ball mill, a wet ball mill, and a pressure emulsifier.
＜炭微粒粉配合ポリ乳酸短繊維の説明＞
本発明の炭微粒粉配合ポリ乳酸短繊維は、黒色着色剤として以下の要件（１）〜（３）を満足する炭微粒粉を繊維の質量に対して０．１〜２０．０質量％配合することを特徴とするものである。
要件（１）：植物由来炭を微粉砕した微粒粉であること
要件（２）：中位径が０．１〜１０μｍの範囲であること
要件（３）：砒素含有量が２ｐｐｍ以下であること
ここで上記の用語の解説および定義について以下に示す。
本発明で用いる炭微粒粉としては備長炭、竹炭、梅炭および活性炭など植物を炭化させた後に微粉砕した植物由来炭であれば特に限定されるものではないが、その用途が化粧料であることを考慮すると、日本国内では日本薬局方（薬用炭）に適合していること、海外ではヨーロッパ規格Ｅ−１５３（Ｖｅｇｅｔａｂｌｅ Ｃａｒｂｏｎ）に適合して入ることが望ましく、炭素含有量が９６％（強熱残分が４％以下）のものを用いる必要がある。また、本発明で用いる炭微粒粉の中位径は、黒顔料の発色性と分散性に影響し、粒子径が小さいと分散性が悪くなり、大きいと発色性が悪く黒色度が低くなる。また炭微粒粉中の次に砒素の含有量であるが、これは粧原基一般試験法又は原子吸光法などの分析方法にて分析した場合に、２ｐｐｍ以下であることが必要である。これにより、より高い安全性が確保できるメリットがある。
<Description of charcoal fine powder blended polylactic acid short fiber>
The charcoal fine particle blended polylactic acid short fiber of the present invention is blended with 0.1 to 20.0% by mass of charcoal fine particle satisfying the following requirements (1) to (3) as a black colorant with respect to the mass of the fiber. It is characterized by doing.
Requirement (1): A fine powder obtained by finely pulverizing plant-derived charcoal Requirement (2): The median diameter is in the range of 0.1 to 10 μm Requirement (3): Arsenic content is 2 ppm or less Here are explanations and definitions of the above terms.
The charcoal fine powder used in the present invention is not particularly limited as long as it is a plant-derived charcoal obtained by carbonizing a plant such as Bincho charcoal, bamboo charcoal, plum charcoal and activated carbon, but its use is a cosmetic. In view of this, it is desirable that it conforms to the Japanese Pharmacopoeia (medicinal charcoal) in Japan, and conforms to European Standard E-153 (Vetable Carbon) overseas, with a carbon content of 96% (strong) It is necessary to use one having a heat residue of 4% or less. Further, the median diameter of the fine carbon powder used in the present invention affects the color developability and dispersibility of the black pigment. If the particle diameter is small, the dispersibility is poor, and if it is large, the color developability is poor and the blackness is low. The arsenic content next to the fine carbon powder is 2 ppm or less when analyzed by an analytical method such as a general test method for makeup bases or an atomic absorption method. Thereby, there is an advantage that higher safety can be secured.
本発明で用いる炭微粒粉の要件としては、上記以外のスペックとして、例えば以下のような規格を満たしていることが好ましい。なお、試験方法としては常法を用いることができ、特に規定のあるものを以下に記載する。このような規格の炭微粒粉を使うことで製品の安全性を高め、品質的に安定した製品を得ることができる。
乾燥減量 １２質量％以下
重金属 ２０ｐｐｍ以下
鉛 ２ｐｐｍ以下
カドミウム １ｐｐｍ以下
水銀 １ｐｐｍ以下
多環芳香族炭化水素類（ＰＡＨｓ） ５０ｐｐｂ以下
なお、乾燥減量の試験方法としては、１２０℃にて４時間乾燥した場合の質量減少を測定したものが挙げられる。多環芳香族炭化水素類（ＰＡＨｓ）の分析は、ガスクロマトグラフィー質量分析機（ＧＣＭＳ）を用いることが好ましい。
As requirements for the fine coal powder used in the present invention, it is preferable that the following specifications are satisfied as specifications other than the above. In addition, a conventional method can be used as the test method, and particularly specified ones are described below. By using such fine carbon powder, it is possible to increase the safety of the product and obtain a product that is stable in quality.
Loss on drying 12 mass% or less Heavy metal 20 ppm or less Lead 2 ppm or less Cadmium 1 ppm or less Mercury 1 ppm or less Polycyclic aromatic hydrocarbons (PAHs) 50 ppb or less As a test method for drying loss, 120 ° C. when dried for 4 hours What measured mass reduction is mentioned. For analysis of polycyclic aromatic hydrocarbons (PAHs), it is preferable to use a gas chromatography mass spectrometer (GCMS).
本発明の炭微粒粉配合ポリ乳酸短繊維は、上記の要件を満足する炭微粒粉を繊維の質量に対して０．１〜２０．０質量％、より好ましくは０．１〜５．０質量％の範囲で配合する。炭微粒粉の配合量が０．１質量％未満では、着色力が足りず着色の効果得られず、２０質量％超では紡糸時に糸切れが発生して繊維が得られない。本発明の炭微粒粉配合ポリ乳酸短繊維は、原料としてポリ乳酸に該炭微粒粉をあらかじめ配合混合しておく他は炭微粒粉未配合のポリ乳酸短繊維と同じ製法で調製できる。なお、予備分散に用いられる分散機としては、単軸押出機、二軸押出機、ニーダー、ロール、乾式ボールミル、湿式ボールミル、加圧乳化装置などが挙げられる。 The carbonic acid fine powder blended polylactic acid short fiber of the present invention is 0.1 to 20.0% by mass, more preferably 0.1 to 5.0% by mass of the fine carbon powder satisfying the above requirements with respect to the mass of the fiber. In the range of%. When the blending amount of the fine carbon powder is less than 0.1% by mass, the coloring power is insufficient and the coloring effect cannot be obtained, and when it exceeds 20% by mass, yarn breakage occurs during spinning and fibers cannot be obtained. The carbonic acid fine powder-blended polylactic acid short fiber of the present invention can be prepared by the same production method as the polylactic acid short fiber not blended with carbon fine powder except that the carbon fine powder is previously blended with polylactic acid as a raw material. Examples of the disperser used for the preliminary dispersion include a single screw extruder, a twin screw extruder, a kneader, a roll, a dry ball mill, a wet ball mill, and a pressure emulsifier.
本発明のポリ乳酸短繊維は、さらに各種の表面処理をすることが可能である。撥水化表面処理の例としては、例えば、メチルハイドロジェンポリシロキサン処理、シリコーンレジン処理、シリコーンガム処理、アクリルシリコーン処理、フッ素化シリコーン処理などのオルガノシロキサン処理、ステアリン酸亜鉛処理などの金属石鹸処理、シランカップリング処理、アルキルシラン処理などのシラン処理、有機チタネート処理、有機アルミネート処理、パーフルオロアルキルシラン、パーフルオロアルキルリン酸エステル塩、パーフルオロポリエーテル処理などのフッ素化合物処理、Ｎ−ラウロイル−Ｌ−リジン処理などのアミノ酸処理などが挙げられ、これらの１種以上を組み合わせて使用することもできる。親水化表面処理の例としては、例えば、寒天処理、デオキシリボ核酸処理、レシチン処理、ポリアクリル酸処理、シリカ処理、アルミナ処理、ジルコニア処理、ポリエーテル変性シラン処理などが挙げられる。 The polylactic acid short fiber of the present invention can be further subjected to various surface treatments. Examples of water repellent surface treatment include, for example, methylhydrogenpolysiloxane treatment, silicone resin treatment, silicone gum treatment, acrylic silicone treatment, organosiloxane treatment such as fluorinated silicone treatment, metal soap treatment such as zinc stearate treatment Silane treatment such as silane coupling treatment, alkyl silane treatment, organic titanate treatment, organic aluminate treatment, perfluoroalkyl silane, perfluoroalkyl phosphate ester salt, fluorine compound treatment such as perfluoropolyether treatment, N-lauroyl Examples include amino acid treatment such as -L-lysine treatment, and one or more of these can also be used in combination. Examples of the hydrophilic surface treatment include agar treatment, deoxyribonucleic acid treatment, lecithin treatment, polyacrylic acid treatment, silica treatment, alumina treatment, zirconia treatment, polyether-modified silane treatment, and the like.
本発明のメークアップ化粧料では、ポリ乳酸短繊維を化粧料に対して０．１〜８０質量％の範囲で配合することが好ましい。特に短繊維を睫毛、眉毛などの毛髪や皮膚に固定するため、樹脂類、ワックス類、ゲル化剤と一緒に配合することが好ましい。さらに発色性をより高めるために、他の顔料や色素などと配合したり、紫外線吸収剤や油剤、界面活性剤、フッ素化合物、樹脂、防腐剤、香料、保湿剤、塩類、溶媒、中和剤、ｐＨ調整剤、キレート剤、酸化防止剤、昆虫忌避剤、生活活性成分などの化粧品素材も使用することができる。 In the makeup cosmetic of the present invention, it is preferable to blend polylactic acid short fibers in the range of 0.1 to 80% by mass with respect to the cosmetic. In particular, in order to fix short fibers to hair such as eyelashes and eyebrows and skin, it is preferable to blend them together with resins, waxes and gelling agents. In order to further improve color developability, it can be blended with other pigments and dyes, UV absorbers, oils, surfactants, fluorine compounds, resins, preservatives, fragrances, moisturizers, salts, solvents, neutralizing agents Cosmetic materials such as pH adjusters, chelating agents, antioxidants, insect repellents, and life-active ingredients can also be used.
ここで言うメークアップ化粧料としては、例えば、ファンデーション、マスカラ、アイライナー、アイブロウ、チーク、コンシーラー、アイシャドウ、ヘアカラー、ヘアマスカラなどが挙げられるが、着色剤未配合のポリ乳酸短繊維は特にファンデーションが、黒色ポリ乳酸短繊維は特にマスカラが好適である。また、剤型は粉体、乳液状、クリーム状、多層分離型、油性等の各種剤型が使用可能である。 Examples of the makeup cosmetics mentioned here include foundations, mascara, eyeliner, eyebrow, teak, concealer, eye shadow, hair color, hair mascara, etc. Mascara is particularly suitable for the black polylactic acid short fiber having a foundation. As the dosage form, various dosage forms such as powder, emulsion, cream, multilayer separation type and oily type can be used.
次に、実施例を挙げ、適宜に図面を用いて本発明のポリ乳酸短繊維及びそれを含有するメークアップ化粧料を詳細に説明するが、本発明は以下に述べる実施例に限定されるものではない。なお、ポリ乳酸短繊維及びこれを黒色に着色した黒色ポリ乳酸短繊維の製造に係る実施例を「製造実施例」と称し、製造実施例で得られたポリ乳酸短繊維及び黒色ポリ乳酸短繊維を配合した化粧料に係る実施例を単に「実施例」と称することとする。 Next, examples will be given, and the polylactic acid short fibers of the present invention and makeup cosmetics containing the same will be described in detail with reference to the drawings as appropriate. However, the present invention is limited to the examples described below. is not. In addition, the example which concerns on manufacture of the polylactic acid short fiber and the black polylactic acid short fiber which colored this black is called a "manufacturing example", and the polylactic acid short fiber and black polylactic acid short fiber which were obtained in the manufacture example An example relating to a cosmetic containing the above will be simply referred to as “Example”.
〔製造実施例１：ポリ乳酸短繊維〕
生分解性ポリマーとしてポリ乳酸（ユニチカ社製 テラマックＴＰ‐４０００ＣＮ）を溶融紡糸機にて、Ｙ型の口金ノズルを通して太さ１０デニール（３５μｍ）の繊維を得た。これを裁断機にて長さ２ｍｍに揃え、目的とするポリ乳酸短繊維を得た。得られた短繊維の走査型電子顕微鏡写真を図１に示す。
[Production Example 1: Polylactic acid short fiber]
Polylactic acid (Terramac TP-4000CN manufactured by Unitika Co., Ltd.) as a biodegradable polymer was obtained with a melt spinning machine through a Y-type nozzle nozzle to obtain a fiber having a thickness of 10 denier (35 μm). This was aligned to a length of 2 mm with a cutting machine to obtain a target polylactic acid short fiber. A scanning electron micrograph of the obtained short fiber is shown in FIG.
〔製造実施例２：カーボンブラック配合ポリ乳酸短繊維〕
１）ファーネス法で製造された、２）比表面積が２１２ｍ２／ｇであって、３）砒素含有量が３ｐｐｍ以下であるカーボンブラック（大東化成工業社製 ＤＫ ＢＬＡＣＫ Ｎｏ．２）０．８質量％とポリ乳酸（ユニチカ製 テラマックＴＰ‐４０００ＣＮ）９９．２質量％を粗混合し、次いで２軸型エクストルーダーを用いて混練し、カーボンブラック混合ペレットを得た。そして、溶融紡糸機に同ペレットを入れ、Ｙ型の口金ノズルを通して太さ１０デニール（３５μｍ）の繊維を得た。これを裁断機にて長さ２ｍｍに揃え、目的とするカーボンブラック配合ポリ乳酸短繊維を得た。得られた短繊維の走査型電子顕微鏡写真を図２に示す。
[Production Example 2: Polylactic acid short fiber containing carbon black]
1) produced by the furnace method, 2) carbon black having a specific surface area of 212 m 2 / g, and 3) arsenic content of 3 ppm or less (DK BLACK No. 2 manufactured by Daito Kasei Kogyo Co., Ltd.) 0.8 mass % And 99.2% by mass of polylactic acid (Terramac TP-4000CN manufactured by Unitika) were roughly mixed and then kneaded using a biaxial extruder to obtain carbon black mixed pellets. Then, the pellets were put into a melt spinning machine, and a fiber having a thickness of 10 denier (35 μm) was obtained through a Y-type nozzle. This was aligned to a length of 2 mm with a cutting machine to obtain a target carbon black-blended polylactic acid short fiber. A scanning electron micrograph of the obtained short fiber is shown in FIG.
〔製造実施例３：黒酸化鉄配合ポリ乳酸短繊維〕
黒酸化鉄（チタン工業社製 タロックスＢＬ−１００Ｐ Ｄ５０＝１．９μｍ）１０．０質量％とポリ乳酸（ユニチカ社製 テラマックＴＰ‐４０００ＣＮ）９０．０質量％を、２台の重量フィーダーを用いて２軸押出機にて溶融混練し、黒酸化鉄混合ペレットを得た。この時、押出機先端に３００ｍｅｓｈスクリーンを装着し分散粒子径を３００ｍｅｓｈパスとした。次いで、溶融紡糸機にて、Ｙ型の口金ノズルを通して太さ１０デニール（３５μｍ）の繊維を得た。これを裁断機にて長さ２ｍｍに揃え、目的とする黒酸化鉄配合ポリ乳酸短繊維を得た。得られた短繊維の走査型電子顕微鏡写真を図３に示す。
[Production Example 3: Polylactic acid short fiber containing black iron oxide]
Black iron oxide (Tarox BL-100P D50 = 1.9 μm manufactured by Titanium Industry Co., Ltd.) 10.0% by mass and polylactic acid (Terramac TP-4000CN manufactured by Unitika Co., Ltd.) 90.0% by mass using two weight feeders The mixture was melt kneaded with a twin screw extruder to obtain black iron oxide mixed pellets. At this time, a 300 mesh screen was attached to the tip of the extruder, and the dispersed particle diameter was set to 300 mesh pass. Subsequently, a fiber having a thickness of 10 denier (35 μm) was obtained through a Y-type nozzle nozzle in a melt spinning machine. This was aligned to a length of 2 mm with a cutting machine to obtain a target black iron oxide-containing polylactic acid short fiber. A scanning electron micrograph of the obtained short fiber is shown in FIG.
〔製造実施例４：表面処理黒酸化鉄配合ポリ乳酸短繊維〕
製造実施例３の黒酸化鉄にオクチルトリエトキシシランを顔料に対して２質量％を予め表面処理し、製造実施例３と同様の方法にて表面処理黒酸化鉄混合ペレットを作製した。次いで溶融紡糸機にて、Ｙ型の口金ノズルを通して太さ１０デニール（３５μｍ）の繊維を得た。これを裁断機にて長さ２ｍｍに揃え、表面処理黒酸化鉄配合ポリ乳酸短繊維を得た。得られた短繊維の走査型電子顕微鏡写真を図４に示す。
[Production Example 4: Polylactic acid short fiber containing surface-treated black iron oxide]
2% by mass of octyltriethoxysilane with respect to the pigment was surface-treated in advance on the black iron oxide of Production Example 3, and surface-treated black iron oxide mixed pellets were produced in the same manner as in Production Example 3. Next, in a melt spinning machine, a fiber having a thickness of 10 denier (35 μm) was obtained through a Y-type nozzle. This was aligned to a length of 2 mm with a cutting machine to obtain a surface-treated black iron oxide-containing polylactic acid short fiber. A scanning electron micrograph of the obtained short fiber is shown in FIG.
〔製造実施例５：炭微粒粉配合ポリ乳酸短繊維〕
炭微粒粉（ラテスト社製 備長炭 ＵＳグレード ＪＭ Ｄ５０＝４．１μｍ）２．０質量％とポリ乳酸（ユニチカ社製 テラマックＴＰ‐４０００ＣＮ）９８．０質量％を、２台の重量フィーダーを用いて２軸押出機にて溶融混練し、炭微粒粉混合ペレットを得た。この時、押出機先端に３００ｍｅｓｈスクリーンを装着し分散粒子径を３００ｍｅｓｈパスとした。次いで、溶融紡糸機にて、Ｙ型の口金ノズルを通して太さ１０デニール（３５μｍ）の繊維を得た。これを裁断機にて長さ２ｍｍに揃え、目的とする炭微粒粉配合ポリ乳酸短繊維を得た。得られた短繊維の走査型電子顕微鏡写真を図５に示す。
[Production Example 5: Polylactic acid short fiber containing fine carbon powder]
Charcoal fine powder (Bastaga charcoal US grade JM D50 = 4.1 μm) 2.0% by mass and polylactic acid (Terramac TP-4000CN, unitika Ltd.) 98.0% by mass using two weight feeders The mixture was melt-kneaded with a twin-screw extruder to obtain a charcoal fine particle mixed pellet. At this time, a 300 mesh screen was attached to the tip of the extruder, and the dispersed particle diameter was set to 300 mesh pass. Subsequently, a fiber having a thickness of 10 denier (35 μm) was obtained through a Y-type nozzle nozzle in a melt spinning machine. This was aligned to a length of 2 mm with a cutting machine, and the intended charcoal fine particle blended polylactic acid short fiber was obtained. A scanning electron micrograph of the obtained short fiber is shown in FIG.
〔製造実施例６：ポリ乳酸短繊維〕
生分解性ポリマーとしてポリ乳酸（ユニチカ社製 テラマックＴＰ−４０００ＣＮ）を溶融紡糸機にて、丸型の口金ノズルを通して太さ５デニール（２４μｍ）の繊維を得た。これを裁断機にて長さ３ｍｍに揃え、目的とするポリ乳酸短繊維を得た。得られた短繊維をデジタルマイクロスコープ（キーエンス社製のＶＨＸ−１００Ｆ）を用いて撮影した外観写真を図７（ａ）に示す。
[Production Example 6: Polylactic acid short fiber]
Polylactic acid (Terramac TP-4000CN manufactured by Unitika Ltd.) as a biodegradable polymer was obtained by a melt spinning machine through a round nozzle nozzle to obtain a fiber having a thickness of 5 denier (24 μm). This was aligned to a length of 3 mm with a cutting machine to obtain a target polylactic acid short fiber. FIG. 7A shows an appearance photograph of the obtained short fibers taken using a digital microscope (VHX-100F manufactured by Keyence Corporation).
〔製造実施例７：ポリ乳酸短繊維〕
生分解性ポリマーとしてポリ乳酸（ユニチカ社製 テラマックＴＰ−４０００ＣＮ）を溶融紡糸機にて、丸型の口金ノズルを通して太さ１０デニール（３５μｍ）の繊維を得た。これを裁断機にて長さ４ｍｍに揃え、目的とするポリ乳酸短繊維を得た。得られた短繊維をデジタルマイクロスコープを用いて撮影した外観写真を図８（ａ）に示す。
[Production Example 7: Polylactic acid short fiber]
Polylactic acid (Terramac TP-4000CN manufactured by Unitika Co., Ltd.) as a biodegradable polymer was obtained with a melt spinning machine through a round nozzle nozzle to obtain a fiber having a thickness of 10 denier (35 μm). This was aligned to a length of 4 mm with a cutting machine to obtain a target polylactic acid short fiber. FIG. 8A shows an appearance photograph of the obtained short fibers taken using a digital microscope.
〔製造実施例８：ポリ乳酸短繊維〕
生分解性ポリマーとしてポリ乳酸（ユニチカ社製 テラマックＴＰ‐４０００ＣＮ）を溶融紡糸機にて、Ｙ型の口金ノズルを通して太さ１０デニール（３５μｍ）の繊維を得た。これを裁断機にて長さ２ｍｍに揃え、目的とするポリ乳酸短繊維を得た。得られた短繊維をデジタルマイクロスコープを用いて撮影した外観写真を図９（ａ）に示す。
[Production Example 8: Polylactic acid short fiber]
Polylactic acid (Terramac TP-4000CN manufactured by Unitika Co., Ltd.) as a biodegradable polymer was obtained with a melt spinning machine through a Y-type nozzle nozzle to obtain a fiber having a thickness of 10 denier (35 μm). This was aligned to a length of 2 mm with a cutting machine to obtain a target polylactic acid short fiber. FIG. 9A shows an appearance photograph of the obtained short fibers taken using a digital microscope.
〔製造比較例1：ポリイミド−アミド短繊維〕
Ｋｅｒｍｅｌ社によりＫｅｒｍｅｌの名称で市販されている、２ｍｍの剛直な直線性を示すポリイミド−アミド繊維。断面形状は三角形。２．２デニール。デジタルマイクロスコープを用いて撮影した外観写真を図１０（ａ）に示す。
[Production Comparative Example 1: Polyimide-amide short fiber]
Polyimide-amide fiber with a rigid linearity of 2 mm, marketed by Kermel under the name Kermel. The cross-sectional shape is a triangle. 2.2 Denier. An appearance photograph taken using a digital microscope is shown in FIG.
〔実施例１：パウダーファンデーション〕
表１の処方と製造方法に従ってパウダーファンデーションを得た。なお、表中の単位は質量％である。
[Example 1: Powder foundation]
A powder foundation was obtained according to the formulation and production method shown in Table 1. In addition, the unit in a table | surface is the mass%.
成分Ａを粗混合した後、均一に溶解した成分Ｂを加えて良く攪拌した後に、容器に充填して製品を得た。
After roughly mixing component A, uniformly dissolved component B was added and stirred well, and then filled into a container to obtain a product.
〔比較例１：パウダーファンデーション〕
実施例１で用いた表１中における製造実施例１のポリ乳酸短繊維を、ＳＩ０１−２ タルクＪＡ−４６ＲJに置き代えた他は全て実施例１と同様にしてパウダーファンデーションを得た。
[Comparative Example 1: Powder Foundation]
A powder foundation was obtained in the same manner as in Example 1 except that the polylactic acid short fibers of Production Example 1 in Table 1 used in Example 1 were replaced with SI01-2 talc JA-46RJ.
〔比較例２：パウダーファンデーション〕
製造実施例１で用いたポリ乳酸の代わりナイロン６を用いた他は全て製造実施例１と同様にしてナイロン短繊維を製造した。実施例１で用いた表１中におけるポリ乳酸短繊維の代わりに、このナイロン短繊維を用いた他は全て実施例１と同様にしてパウダーファンデーションを得た。
[Comparative Example 2: Powder Foundation]
Nylon short fibers were produced in the same manner as in Production Example 1 except that nylon 6 was used instead of the polylactic acid used in Production Example 1. A powder foundation was obtained in the same manner as in Example 1 except that this nylon short fiber was used instead of the polylactic acid short fiber in Table 1 used in Example 1.
（パウダーファンデーションの評価）
女性パネラー１０名に、パウダーファンデーションを使用してもらい、透明感、素肌感、均一な化粧仕上がりをアンケート形式で回答してもらった。評価が悪い場合を０点、評価が良い場合を５点とし、パネラーの平均点数で評価結果とした。したがって点数が高いほど評価が優れていることを示している。結果を表２に示す。
(Evaluation of powder foundation)
Ten female panelists used a powder foundation and asked them to respond in a questionnaire format with a sense of transparency, bare skin, and a uniform makeup finish. When the evaluation was poor, 0 points were given, and when the evaluation was good, 5 points, and the average score of the panelists was used as the evaluation result. Therefore, the higher the score, the better the evaluation. The results are shown in Table 2.
表２の結果から、製造実施例１のポリ乳酸短繊維をパウダーファンデーションに配合した実施例１は、未配合の比較例１及びナイロン短繊維を配合している比較例２と比較して、透明感、素肌感、均一な化粧仕上がりの効果に優れており、より肌の肌理を再現できることが判る。また、実施例１のものは、生分解性ポリマー素材を配合しているので比較例１及び２のものよりも環境にやさしい。 From the results shown in Table 2, Example 1 in which the polylactic acid short fibers of Production Example 1 were blended in the powder foundation was more transparent than Comparative Example 1 in which the unblended Comparative Example 1 and nylon short fibers were blended. It is excellent in feeling, bare skin feeling and uniform makeup finish, and it can be seen that the texture of the skin can be reproduced more. Moreover, since the thing of Example 1 mix | blends the biodegradable polymer raw material, it is environmentally friendly rather than the thing of Comparative Examples 1 and 2.
〔実施例２：マスカラ〕
製造実施例２のカーボンブラック配合ポリ乳酸短繊維を用い、表３の処方と製造方法に従ってマスカラを得た。なお、表中の単位は質量％である。
[Example 2: Mascara]
Using the carbon black blended polylactic acid short fibers of Production Example 2, mascara was obtained according to the formulation and production method shown in Table 3. In addition, the unit in a table | surface is the mass%.
成分Ｂを８０℃で均一に溶解した成分Ａに加えた。次いで、成分Ｃも８０℃で均一に混合し、成分Ａに徐々に加えてよく混合した。攪拌下で徐冷して液温が３０℃になったところで成分Ｄを加え、最後に成分Ｅを加えてよく混合した後、ブラシつき容器に充填して製品を得た。
Component B was added to Component A, which was uniformly dissolved at 80 ° C. Next, component C was also uniformly mixed at 80 ° C., and gradually added to component A and mixed well. When the liquid temperature reached 30 ° C. while stirring, the component D was added. Finally, the component E was added and mixed well, and then filled into a container with a brush to obtain a product.
〔実施例３：マスカラ〕
実施例２で用いた製造実施例２のカーボンブラック配合ポリ乳酸短繊維の代わりに製造実施例３の黒酸化鉄配合ポリ乳酸短繊維を用いた他は全て実施例２と同様にして製品を得た。
[Example 3: Mascara]
A product was obtained in the same manner as in Example 2 except that the black iron oxide-containing polylactic acid short fiber of Production Example 3 was used instead of the carbon black-containing polylactic acid short fiber of Production Example 2 used in Example 2. It was.
〔実施例４：マスカラ〕
実施例２で用いた製造実施例２のカーボンブラック配合ポリ乳酸短繊維の代わりに製造実施例４の表面処理黒酸化鉄配合ポリ乳酸短繊維を用いた他は全て実施例２と同様にして製品を得た。
[Example 4: mascara]
Product in the same manner as in Example 2 except that the surface-treated black iron oxide-containing polylactic acid short fiber of Production Example 4 was used instead of the carbon black-containing polylactic acid short fiber of Production Example 2 used in Example 2. Got.
〔実施例５：マスカラ〕
実施例２で用いた製造実施例２のカーボンブラック配合ポリ乳酸短繊維の代わりに製造実施例５の炭微粒粉配合ポリ乳酸短繊維を用いた他は全て実施例２と同様にして製品を得た。
[Example 5: mascara]
A product was obtained in the same manner as in Example 2, except that the carbon black-blended polylactic acid short fibers of Production Example 2 used in Example 2 were replaced with the carbon fine particle-blended polylactic acid short fibers of Production Example 5. It was.
〔比較例３：マスカラ〕
実施例２においてカーボンブラック配合ポリ乳酸短繊維を精製水に置き代えた他は全て実施例２と同様にして製品を得た。
[Comparative Example 3: Mascara]
A product was obtained in the same manner as in Example 2 except that the carbon black-blended polylactic acid short fibers were replaced with purified water in Example 2.
〔比較例４：マスカラ〕
製造実施例２で用いたカーボンブラックの代わりに比表面積が４００ｍ２／ｇのカーボンブラックを用いた他は全て製造実施例２と同様にしてカーボンブラック配合ポリ乳酸短繊維を製造した。実施例２で用いたカーボンブラック配合ポリ乳酸短繊維の代わりに、このカーボンブラック配合ポリ乳酸短繊維を用いた他は全て実施例２と同様にして製品を得た。
[Comparative Example 4: Mascara]
A carbon black-containing polylactic acid short fiber was produced in the same manner as in Production Example 2 except that carbon black having a specific surface area of 400 m 2 / g was used instead of the carbon black used in Production Example 2. A product was obtained in the same manner as in Example 2 except that this carbon black-containing polylactic acid short fiber was used instead of the carbon black-containing polylactic acid short fiber used in Example 2.
（マスカラの評価）
上記パウダーファンデーションの評価方法と同様の方法でマスカラの評価を行った。結果を表４に示す。
(Evaluation of mascara)
Mascara was evaluated by the same method as the above powder foundation evaluation method. The results are shown in Table 4.
表４の結果から、本発明の実施例は比較例に比べて各評価項目で優れた特性を示していることが判る。一方、比較例３は、短繊維未配合のものであるが、全体的に評価が劣っていることが判る。比較例４は、比表面積が大きなカーボンブラックを使用した場合の例であるが、やや塗布しにくかったため、使用感が悪く、他の評価項目も悪くなった。また、本発明の実施例は、生分解性ポリマー素材を配合しているので環境にやさしい。 From the results of Table 4, it can be seen that the examples of the present invention show superior characteristics in each evaluation item as compared with the comparative examples. On the other hand, although the comparative example 3 is a thing without a short fiber combination, it turns out that evaluation is inferior generally. Comparative Example 4 is an example where carbon black having a large specific surface area was used, but it was somewhat difficult to apply, so the usability was poor and other evaluation items were also poor. Moreover, since the Example of this invention mix | blends the biodegradable polymer raw material, it is environmentally friendly.
表４の結果から、本発明のマスカラは塗りやすく、睫毛が長く見える効果（ボリューム感の付与効果）に優れていたが、この効果が発現している機構について詳細に調べた結果を以下に示す。 From the results of Table 4, the mascara of the present invention was easy to apply and was excellent in the effect that the eyelashes look long (the effect of imparting a feeling of volume). The results of detailed examination of the mechanism in which this effect is manifested are shown below. .
〔実施例６〜８、比較例５：マスカラ〕
ポリ乳酸短繊維の形状維持機能の確認
実施例２のマスカラ及び、表３の処方と製造方法を準用し、成分Ｅのカーボンブラック配合ポリ乳酸短繊維を製造実施例６〜８に記載のポリ乳酸短繊維に置換した場合のマスカラ（実施例６〜８）を用い、その形状維持機能を以下の方法により評価した結果をそれぞれ図６〜９に、また、特許文献５にあるような剛直な繊維を用いた場合（製造比較例１を用いた比較例５）の評価結果を図１０に示す。
[Examples 6 to 8, Comparative Example 5: Mascara]
Confirmation of the shape maintaining function of the polylactic acid short fiber The mascara of Example 2 and the formulation and production method of Table 3 were applied mutatis mutandis to produce the carbon black-blended polylactic acid short fiber of Component E. Polylactic acid described in Examples 6-8 Using mascara (Examples 6 to 8) when substituted with short fibers, the results of evaluating the shape maintenance function by the following method are shown in FIGS. 6 to 9 and rigid fibers as in Patent Document 5, respectively. FIG. 10 shows the results of evaluation in the case of using (Comparative Example 5 using Production Comparative Example 1).
＜評価方法および結果＞
デジタルマイクロスコープ（キーエンス社製ＶＨＸ−１００Ｆ、倍率５０倍）を用いて下記条件で観察を行った。図６〜１０の（ａ）は、製造実施例２及び６〜８と製造比較例１の短繊維を大気中で黒色プラスチック板に載せて撮影した際の外観写真である。図６〜１０の（ｂ）は、マスカラ容器内における、製剤中の短繊維のマスカラの塗布具（マスカラブラシ）への絡みつきやすさと、その時の形状を確認する目的で、マスカラブラシ表面の短繊維の状態を撮影した際の外観写真の拡大像である。図６〜１０の（ｃ）は、睫毛へマスカラを塗布した後の短繊維の形状を確認する目的で、睫毛モデル（ビューラックス社製）に塗布したものを撮影した際の外観写真である。
<Evaluation method and results>
Observation was performed under the following conditions using a digital microscope (VHX-100F manufactured by Keyence Corporation, magnification 50 times). (A) of FIGS. 6-10 is an external appearance photograph when the short fibers of Production Examples 2 and 6-8 and Production Comparative Example 1 are photographed on a black plastic plate in the atmosphere. (B) in FIGS. 6 to 10 show the short fibers on the surface of the mascara brush for the purpose of confirming the ease of entanglement of the short fibers in the preparation with the mascara applicator (mascara brush) and the shape at that time in the mascara container. It is a magnified image of the appearance photograph at the time of photographing the state of. (C) of FIGS. 6-10 is an external appearance photograph when what was applied to the eyelash model (manufactured by Beaulux) was photographed for the purpose of confirming the shape of the short fiber after applying mascara to the eyelashes.
図６〜１０の（ａ）を見ると、いずれも良好な直線状の形状を有していることが判る。従って、繊維本来の空気中での安定な形状はいずれも直線状であると言える。
図６〜９の（ｂ）に示す本発明の実施例では、いずれも製剤中のマスカラブラシ表面では、短繊維は直線性を失い、曲がってブラシに絡みついている様子が観察される。これに対して図１０（ｂ）の剛直な繊維を配合した比較例５では、ブラシ表面でも直線性を維持していることが判る。マスカラ容器内には、余分な製剤を落として、適切な量を塗布するためのシゴキ部が設置されており、剛直な繊維は一般的なシゴキ部を持つ容器では、本発明のような形状維持機能を有している短繊維と比較して、マスカラブラシへの絡みつきが弱い分、より多くしごかれてしまうことが予想される。図６〜１０の（ｃ）では、いずれも繊維の形状は直線状を示していることから、差が生じる原因の１つとして、マスカラブラシに付いてくる短繊維の量が違うことが考えられる。
6 (a) to 10 (a), it can be seen that all have a good linear shape. Accordingly, it can be said that all of the stable shapes of the fibers in the air are linear.
In the examples of the present invention shown in FIGS. 6 to 9B, it is observed that the short fibers lose their linearity and are bent and entangled with the brush on the surface of the mascara brush in the preparation. In contrast, in Comparative Example 5 in which the rigid fibers in FIG. 10B are blended, it can be seen that the linearity is maintained even on the brush surface. In the mascara container, there is a squirrel part for dropping an extra formulation and applying an appropriate amount, and the rigid fiber is in the shape of the present invention in a container having a general scouring part. Compared with the short fiber which has a function, it is anticipated that it will be squeezed more by the part with the weak entanglement in a mascara brush. In each of FIGS. 6 to 10 (c), since the shape of the fibers is linear, one of the causes of the difference is considered to be that the amount of short fibers attached to the mascara brush is different. .
また、図６〜１０の（ｃ）の短繊維の付着形状を良く観察すると、図１０（ｃ）では、繊維が睫毛の繊維の向きからかなり曲がってついているものが観察されている。そこで、実際にパネラーを用いて、実施例２及び実施例６〜８と比較例５について以下のように、使用試験を実施し、短繊維の付着状態を観察した。その結果を表５に示す。 Moreover, when the adhesion shape of the short fiber of FIGS. 6-10 (c) is observed well, in FIG. 10 (c), it is observed that the fiber is bent considerably from the direction of the eyelash fiber. Therefore, using a paneler, a usage test was conducted on Example 2 and Examples 6 to 8 and Comparative Example 5 as follows, and the adhesion state of the short fibers was observed. The results are shown in Table 5.
＜短繊維の睫毛への付着状態の観察＞
パネラー１０名を用いて、試料を一般的なマスカラの塗布方法により塗布してもらい、塗布直後の繊維が、睫毛の長軸方向に対して揃っているか否かを目視で確認した。評価は、専門の判定員が短繊維が睫毛の方向に揃っているか否かを判定し、揃っていると判定されたパネラーの人数を以て行った。結果を表５に示す。
<Observation of short fibers attached to eyelashes>
Using 10 panelists, the sample was applied by a general mascara application method, and it was visually confirmed whether or not the fibers immediately after application were aligned in the major axis direction of the eyelashes. The evaluation was performed by the number of panelists who judged that a specialized judge judged whether or not the short fibers were aligned in the direction of the eyelashes. The results are shown in Table 5.
表５の結果より、実施例２および実施例６〜８では、短繊維が良くそろっており、大変美しい形状となっていたのに対し、比較例５では、睫毛に対して横向きや斜め向きのものが存在し、実施例と比較して外観上の差異が大きかった。前記モデル系での試験結果とヒトでの試験結果で同じ傾向が得られたことから、本発明の短繊維は、マスカラブラシから睫毛に塗布された後、形状が直線状に戻る過程で、睫毛に沿って戻りやすい特性を有しているものと思われる。 From the results shown in Table 5, in Example 2 and Examples 6-8, the short fibers were well aligned and had a very beautiful shape, whereas in Comparative Example 5, the fibers were laterally or obliquely oriented with respect to the eyelashes. There was a large difference in appearance compared to the examples. Since the same tendency was obtained between the test results in the model system and the test results in humans, the short fibers of the present invention were applied to the eyelashes from the mascara brush, and then the shape of the eyelashes returned to the linear shape. It seems that it has the characteristic that it is easy to return along.
本発明のポリ乳酸短繊維は、環境への負荷が小さく、睫毛や眉毛にボリューム感を付与でき、肌の肌理を再現できるなどの美しい仕上がりのメークアップ化粧料を得ることができ、かつポリ乳酸短繊維の持つ優れた形状維持機能を利用することにより、化粧料使用後は直線状の形状になり化粧効果を高めながら、マスカラブラシなど化粧料塗布具には変形してより多くの繊維が付着できるため、睫毛や眉毛にボリューム感を付与する効果がより高く得られるので、産業上の利用効果が大である。
The polylactic acid short fiber of the present invention has a small environmental load, can give a voluminous feel to the eyelashes and eyebrows, can reproduce the texture of the skin, and can produce a beautifully finished makeup cosmetic. By using the excellent shape maintenance function of short fibers, it becomes a linear shape after using cosmetics and enhances the makeup effect, while deforming cosmetic cosmetic applicators such as mascara brush and attaching more fibers Therefore, the effect of imparting a sense of volume to the eyelashes and eyebrows can be obtained higher, and the industrial utilization effect is great.
Claims (1)
以下の要件（１）〜（３）を満足する炭微粒粉を繊維の質量に対して０．１〜２０．０質量％配合することを特徴とするポリ乳酸短繊維。
要件（１）：植物由来炭を微粉砕した微粒粉であること
要件（２）：中位径が０．１〜１０μｍの範囲であること
要件（３）：砒素含有量が２ｐｐｍ以下であること Fiber length is 0.1~10.0mm, fiber diameter Ri Oh in 0.5 to 20 denier,
Following requirements (1) to (3) a polylactic acid staple fibers charcoal fine powder satisfying characterized that you blending from 0.1 to 20.0% by weight, based on the weight of the fibers.
Requirement (1): Finely pulverized plant-derived charcoal
Requirement (2): The median diameter is in the range of 0.1 to 10 μm.
Requirement (3): Arsenic content is 2 ppm or less
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| JP2007039861A (en) * | 2005-06-29 | 2007-02-15 | Daito Kasei Kogyo Kk | Black-colored short fiber and blended cosmetic |
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