JP2020075898A - Liquid cosmetics - Google Patents

Liquid cosmetics Download PDF

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JP2020075898A
JP2020075898A JP2018211530A JP2018211530A JP2020075898A JP 2020075898 A JP2020075898 A JP 2020075898A JP 2018211530 A JP2018211530 A JP 2018211530A JP 2018211530 A JP2018211530 A JP 2018211530A JP 2020075898 A JP2020075898 A JP 2020075898A
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liquid
oily substance
oily
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mass
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JP7365030B2 (en
JP2020075898A5 (en
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恭史 西尾
Yashishi Nishio
恭史 西尾
素勉 池田
Motoyasu IKEDA
素勉 池田
清水 徹
Toru Shimizu
徹 清水
將義 久間
Masayoshi Hisama
將義 久間
公男 吉尾
Kimio Yoshio
公男 吉尾
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Toyo Beauty Co Ltd
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Toyo Beauty Co Ltd
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Priority to CN201980073748.5A priority patent/CN112969511B/en
Priority to PCT/JP2019/041700 priority patent/WO2020095700A1/en
Priority to TW108140086A priority patent/TWI830806B/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/31Hydrocarbons
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Chemical & Material Sciences (AREA)
  • Dermatology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Dispersion Chemistry (AREA)
  • Emergency Medicine (AREA)
  • Cosmetics (AREA)

Abstract

To manufacture cosmetics, in which spherical oily scrubs are dispersed, so as to have highly moisturizing properties without stickiness in use, have excellent product aesthetics and usability, and comprise scrubs with vibration stability, as well as are sure to change an oil phase to scrubs.SOLUTION: In a transparent or translucent liquid cosmetic in which oily scrub particles consisting of a liquid oily substance that is liquid at room temperature and a solid oily substance that is solid at room temperature are dispersed in an external water phase, the mass ratio of the liquid oily substance and the solid oily substance is prepared in the range of 1: (0.05-10) to obtain a transparent or translucent liquid cosmetic containing 60% by mass or more of hydrocarbon oil in the liquid oily substance and 60% by mass or more of a higher alcohol in the solid oily substance.SELECTED DRAWING: None

Description

この発明は、液状化粧料に関し、油性スクラブ粒子が外水相に分散して透明または半透明の状態を示す液状化粧料及びその製造方法に関する。   The present invention relates to a liquid cosmetic composition, and more particularly to a liquid cosmetic composition in which oily scrub particles are dispersed in an outer water phase to show a transparent or translucent state, and a method for producing the same.

一般的な透明又は半透明な液状化粧料としては、化粧水、美容液、オールインワンジェル、シャンプーなどが知られているが、これらは経日安定性や製法の制約により均一な外観であり、油剤の配合量を増やすと外観が白色になることから油剤の配合量は低い。   As general transparent or translucent liquid cosmetics, lotion, beauty essence, all-in-one gel, shampoo, etc. are known, but they have a uniform appearance due to the stability over time and the manufacturing method, and an oil solution. The compounding amount of the oil agent is low because the external appearance becomes white when the compounding amount of is increased.

一方で、化粧料として優れた使用感を生み出すためには、油剤の配合を高める必要があり、しかも外観を意図的に不均一にして美観を得る化粧料が求められ、例えば、水相と油相が完全に分離した2層式化粧料や、固形油スクラブを配合した化粧料などが知られている。   On the other hand, in order to produce an excellent feeling of use as a cosmetic, it is necessary to enhance the blending of the oil agent, and further, a cosmetic that intentionally makes the appearance non-uniform to obtain an aesthetic appearance is required. Two-layer type cosmetics in which the phases are completely separated and cosmetics containing solid oil scrub are known.

しかし、2層式化粧料は、容器に充填する際、水相と油相を別々に充填する手間が必要であり、もしくは撹拌をしながら充填可能な特殊な機械を必要とし、さらには低温で油相が融点を下回ると固化することを避けるために、選択可能な油剤の種類が少なく、そのために使用感の改善に充分対応できないという欠点がある。   However, the two-layer type cosmetics require a labor for separately filling the water phase and the oil phase when filling the container, or a special machine capable of filling while stirring, and further, at a low temperature. In order to avoid solidification when the oil phase falls below the melting point, there are a small number of types of oil agents that can be selected, so that there is a drawback that it is not possible to sufficiently deal with improving the feeling of use.

また、化粧料に固形油スクラブを配合する際には、予め固形油をスクラブ化してから配合することが一般に行なわれるが、そのようにするとスクラブ粒子の色や大きさが画一的になって多様な製品の製造が難しく、またスクラブの素材に高融点の油剤を用いると、化粧料を塗布したときに油剤が体温で溶け難く使用感が損なわれるという欠点がある。   In addition, when solid oil scrub is blended into cosmetics, it is generally practiced to scrub the solid oil in advance and then blend it, which makes the color and size of the scrub particles uniform. It is difficult to manufacture various products, and when an oil agent having a high melting point is used as a material for scrub, the oil agent is difficult to melt at body temperature when a cosmetic is applied, and the usability is impaired.

これらの欠点を解消して優れた製品美観と使用性を両立する化粧料となるように、液状油性物質と固形油性物質を混合した半固体油性物質を加温溶解したものを、加温した水溶性増粘剤相に撹拌しながら投入し、さらに撹拌しながら冷却することで、球状スクラブ化した油性成分を分散させることが知られている(特許文献1)。   In order to eliminate these drawbacks and to provide a cosmetic that has both excellent product aesthetics and usability, a semisolid oily substance obtained by mixing a liquid oily substance and a solid oily substance is heated and dissolved in a warm water-soluble solution. It is known that the spherically scrubbed oily component is dispersed by pouring into the thickening agent phase with stirring and further cooling while stirring (Patent Document 1).

特開平4−346909号公報JP-A-4-346909

しかし、上記した従来の手法では、液状油性物質と固形油性物質を任意に配合可能ではなく、選択した油剤の種類によっては油相が球状スクラブ化されなかったり、製造中に水相が白濁する場合があり、その場合には、得られた球状スクラブを一旦回収し、洗浄してから別の水相に投入する工程が必要になる。また、球状スクラブが製造できた場合でも使用時や輸送時の振動によって球状スクラブが崩壊したり粘着凝集する場合があった。   However, in the conventional method described above, it is not possible to arbitrarily mix the liquid oily substance and the solid oily substance, and depending on the type of the selected oil agent, the oil phase is not spherically scrubbed, or the aqueous phase becomes cloudy during production. In that case, a step of once collecting the obtained spherical scrub, washing it, and then throwing it into another aqueous phase is required. Even if the spherical scrub can be manufactured, the spherical scrub may be collapsed or adhered and aggregated due to vibration during use or transportation.

このように従来の球状スクラブを含有する化粧料は、油相が確実にスクラブ化するように製造することが容易でなく、また得られた化粧料に、優れた製品美観と使用性を持たせると共に振動に対する安定性を担保させることが困難であった。   As described above, the conventional cosmetics containing spherical scrubs are not easy to produce so that the oil phase is certainly scrubbed, and the obtained cosmetics have excellent product aesthetics and usability. At the same time, it was difficult to ensure stability against vibration.

そこで、この発明の課題は、上記した問題点を解決して、球状の油性スクラブを分散させた化粧料について、使用状態にべたつき感が無く保湿性の高い、優れた製品美観と使用感を有するものとし、かつスクラブに振動安定性があり、しかも油相が確実にスクラブ化するように製造できることである。   Therefore, an object of the present invention is to solve the above-mentioned problems and to provide a cosmetic in which spherical oily scrubs are dispersed, which has a high moisturizing property without a sticky feeling in a use state, and has an excellent product aesthetics and a feeling of use. In addition, the scrub has vibration stability and can be manufactured so that the oil phase is scrubbed surely.

上記の課題を解決するために、本願の発明者らは、油性物質を乳化せずに分散させることで特徴的な外観を有する化粧料について鋭意研究を重ねた結果、液状油性物質の主な構成油剤を炭化水素油とし、固形油性物質の主な構成油剤を高級アルコールに限定し、かつ液状油性物質と固形油性物質の混合比を所定範囲内にすることによって、安定して均一性の高い球状油性スクラブを得ることができ、しかもスクラブが振動安定性を有するために品質が安定し、かつ使用感を満足させ得る化粧料となることを見出し、この発明を完成させるに至ったのである。   In order to solve the above problems, the inventors of the present application have earnestly studied cosmetics having a characteristic appearance by dispersing an oily substance without emulsifying, and as a result, the main constitution of the liquid oily substance Stable and highly uniform spheres by using hydrocarbon oil as the oil agent, limiting the main oil agent of the solid oily substance to higher alcohols, and keeping the mixing ratio of the liquid oily substance and the solid oily substance within a predetermined range. The inventors have found that an oily scrub can be obtained, and that the scrub has vibration stability, so that the quality is stable and that the cosmetic can satisfy the feeling of use, and has completed the present invention.

すなわち、この発明においては、上記の課題を解決するために、室温で液体の液状油性物質(B)及び室温で固体の固形油性物質(C)の混合物(A)からなる油性スクラブ粒子が外水相に分散している透明または半透明の液状化粧料において、
前記混合物(A)が、質量比で液状油性物質(B):固形油性物質(C)=1:(0.05〜10)の混合物であり、
前記液状油性物質(B)が、炭化水素油を60質量%以上含有し、
前記固形油性物質(C)が、炭素数14以上の高級アルコールを60質量%以上含有することを特徴とする液状化粧料としたのである。
なお、上記した室温とは、日本薬局方で定められる1〜30℃の温度範囲である。
That is, in the present invention, in order to solve the above-mentioned problems, oily scrub particles composed of a mixture (A) of a liquid oily substance (B) which is liquid at room temperature and a solid oily substance (C) which is solid at room temperature are external water. In a transparent or translucent liquid cosmetic that is dispersed in the phase,
The mixture (A) is a mixture of a liquid oily substance (B): solid oily substance (C) = 1: (0.05 to 10) in a mass ratio,
The liquid oily substance (B) contains at least 60 mass% of hydrocarbon oil,
The solid oily substance (C) is a liquid cosmetic characterized by containing 60% by mass or more of a higher alcohol having 14 or more carbon atoms.
In addition, the above-mentioned room temperature is a temperature range of 1 to 30 ° C. determined by the Japanese Pharmacopoeia.

上記炭化水素油としては、スクワラン、α‐オレフィンオリゴマー、流動パラフィンから選ばれる1種以上の炭化水素油を用いることが好ましい。
また、上記固形油性物質としては、セタノール、ベヘニルアルコール、水添ナタネ油アルコール、ステアリルアルコールから選ばれる1種以上の固形油性物質であることが好ましい。
As the above-mentioned hydrocarbon oil, it is preferable to use one or more kinds of hydrocarbon oil selected from squalane, α-olefin oligomer and liquid paraffin.
The solid oily substance is preferably one or more solid oily substances selected from cetanol, behenyl alcohol, hydrogenated rapeseed oil alcohol and stearyl alcohol.

上記したように構成されるこの発明に係る液状化粧料は、油性スクラブ粒子を構成する成分である液状油性物質と固形油性物質の主構成油剤を、所定量の炭化水素油と高級アルコールからなり、かつ液状油性物質と固形油性物質の配合比を所定割合にしたので、油性スクラブ粒子径が適度な大きさで揃っていて粒度分布にバラつきが少なく、かつ均一分散した液状化粧料になる。そのため、均質な性状が実感される優れた製品美観を有し、透明あるいは半透明化粧料であっても比較的多量の油剤を配合可能になり、優れた使用感を有し、さらに油性スクラブ粒子が、振動安定性に優れていて長時間の流通や保存にも耐える品質安定性をも備えた化粧料になる。   The liquid cosmetic according to the present invention configured as described above comprises a main constituent oil agent of a liquid oily substance and a solid oily substance which are components constituting oily scrub particles, and is composed of a predetermined amount of hydrocarbon oil and higher alcohol, In addition, since the mixing ratio of the liquid oily substance and the solid oily substance is set to a predetermined ratio, the oily scrub particles have a proper size and are uniform in size, and there is little variation in particle size distribution, and a liquid cosmetic composition is uniformly dispersed. Therefore, it has an excellent product aesthetic that a homogeneous property is actually felt, and even a transparent or translucent cosmetic can be blended with a relatively large amount of an oil agent, which has an excellent usability and further has an oily scrub particle. However, it is a cosmetic with excellent vibration stability and quality stability that can withstand long-term distribution and storage.

上記のような優れた特徴をより確実に奏する化粧料とするために、油性スクラブ粒子が化粧料100質量%中に0.3〜5.0質量%配合される化粧料とすることが好ましい。   In order to provide a cosmetic that more reliably exhibits the above-described excellent characteristics, it is preferable to use a cosmetic in which 0.3 to 5.0% by mass of oily scrub particles are mixed in 100% by mass of the cosmetic.

さらに、上記のような優れた特徴をより確実に奏する化粧料とするためには、外水相に分散している油性スクラブ粒子の平均粒子径が0.2〜2.0mmである化粧料とすることが好ましい。   Furthermore, in order to more reliably provide the above-described excellent characteristics, a cosmetic in which the average particle size of the oily scrub particles dispersed in the outer water phase is 0.2 to 2.0 mm, Preferably.

さらに、上記のような優れた特徴をより確実に奏する化粧料を製造するために、室温で液体の液状油性物質(B)及び室温で固体の固形油性物質(C)の混合物(A)を60〜80℃に加熱して溶解させ、次いで60〜80℃に加熱した水相に投入し、攪拌して前記混合物(A)を球状化した後、冷却して油性スクラブ粒子が外水相に均一分散した透明または半透明の液状化粧料を得る工程からなり、上記(A)、(B)、(C)の配合成分の要件を備えた液状化粧料の製造方法とすることが好ましい。   Furthermore, in order to produce a cosmetic material that more reliably exhibits the above-mentioned excellent characteristics, a mixture (A) of a liquid oily substance (B) which is liquid at room temperature and a solid oily substance (C) which is solid at room temperature is mixed with 60 Heated to -80 ° C to dissolve, then put into an aqueous phase heated to 60 to 80 ° C, stirred to spheroidize the mixture (A), and then cooled to uniformly disperse the oily scrub particles in the external aqueous phase. It is preferable to provide a method for producing a liquid cosmetic which comprises a step of obtaining a dispersed transparent or translucent liquid cosmetic, and which satisfies the requirements for the compounding ingredients (A), (B) and (C) described above.

前記攪拌する際には、混合機、分散機、混練機、ホモミキサー、圧力式ホモジナイザーまたは高速攪拌機を用いて粒子径を均一化するように攪拌することが好ましい。   At the time of stirring, it is preferable to use a mixer, a disperser, a kneader, a homomixer, a pressure homogenizer or a high-speed stirrer so as to make the particle diameter uniform.

この発明は、所定の混合物からなる油性スクラブ粒子が外水相に分散している液状化粧料であって、混合物の液状油性物質と固形油性物質の成分及び配合割合を所定範囲に調製したので、適度な大きさの球状スクラブが分散することで優れた製品美観を有し、透明化粧料にもかかわらず多量の油剤を配合することで優れた使用感を有し、さらにはスクラブが振動安定性を有し、優れた品質安定性を有する化粧料となる利点がある。   This invention is a liquid cosmetic in which oily scrub particles consisting of a predetermined mixture are dispersed in the outer aqueous phase, and since the components and the blending ratio of the liquid oily substance and the solid oily substance of the mixture are adjusted to be within a predetermined range, It has an excellent product aesthetic by dispersing spherical scrubs of appropriate size, and it has an excellent feeling of use by blending a large amount of oil agent despite the fact that it is a transparent cosmetic. And has the advantage of being a cosmetic having excellent quality stability.

また、この発明の製造方法では、上記のような優れた特徴を奏する化粧料を効率よく安定した品質で製造できる利点がある。   Further, the production method of the present invention has an advantage that a cosmetic having the above-mentioned excellent characteristics can be efficiently produced with stable quality.

実施例4及び実施例5の化粧水をそれぞれ充填した透明容器を左右に並べて示す図面代用写真Drawing-substituting photographs showing the transparent containers of Example 4 and Example 5 each filled with the lotion side by side. 比較例6及び比較例7の化粧水をそれぞれ充填した透明容器を左右に並べて示す図面代用写真Drawing-substituting photographs showing the transparent containers in Comparative Examples 6 and 7 which are filled with the lotions, respectively, arranged side by side. 実施例15の化粧水中の油性スクラブ粒子を示す図面代用の顕微鏡写真A micrograph, as a substitute for a drawing, showing the oily scrub particles in the lotion of Example 15. 実施例16の化粧水中の油性スクラブ粒子を示す図面代用の顕微鏡写真A micrograph, as a substitute for a drawing, showing the oily scrub particles in the lotion of Example 16.

この発明の実施形態の液状化粧料は、室温で液体であり「炭化水素油を60質量%以上含有する液状油性物質(B)」及び室温で固体であり「炭素数14以上の高級アルコールを60質量%以上含有する固形油性物質(C)」を「所定の割合で配合した混合物(A)」からなる油性スクラブ粒子を、外水相に分散させた透明または半透明の液状化粧料である。   The liquid cosmetic of the embodiment of the present invention is a liquid at room temperature and is a "liquid oily substance (B) containing 60% by mass or more of hydrocarbon oil" and a solid at room temperature "60 higher alcohols having 14 or more carbon atoms. A transparent or semi-transparent liquid cosmetic in which oily scrub particles consisting of a "mixture (A)" containing "a solid oily substance (C) contained in an amount of at least mass% in a predetermined ratio" are dispersed in an external water phase.

この発明における液状油性物質(B)は、室温、例えば25℃で液体であり、通常の化粧料に配合される皮膚に無害な炭化水素類、エーテル類、エステル類、高級アルコール類、脂肪酸類、植物油類、シリコーン油類などを好適に用いることができる。   The liquid oily substance (B) in the present invention is a liquid at room temperature, for example, 25 ° C, and is a hydrocarbon harmless to the skin, ethers, esters, higher alcohols, fatty acids, which are harmless to the skin, which are mixed in ordinary cosmetics. Vegetable oils and silicone oils can be preferably used.

このような液状油性物質の具体例としては、炭化水素類として、流動パラフィン、α‐オレフィンオリゴマーおよびスクワランなどが挙げられる。また、エーテル類として、ジオクチルエーテル、エチレングリコールモノラウリルエーテル、エチレングリコールジオクチルエーテルおよびグリセロールモノオレイルエーテルなどが挙げられ、エステル類として、トリ2‐エチルヘキサン酸グリセリル、2‐エチルヘキサン酸セチル、イソノナン酸イソノニル、イソノナン酸イソトリデシル、ミリスチン酸イソプロピル、ミリスチン酸ブチル、ミリスチン酸オクチルドデシル、パルミチン酸イソプロピル、ステアリン酸エチル、パルミチン酸オクチル、イソステアリン酸イソセチル、ステアリン酸ブチル、リノール酸エチル、リノール酸イソプロピル、オレイン酸エチル、ミリスチン酸イソセチル、ミリスチン酸イソステアリル、パルミチン酸イソステアリル、パルミチン酸セチル、トリイソステアリン酸トリメチロールプロパン、テトラ2‐エチルヘキサン酸ペンタエリスリトール、カプリル酸セチル、ラウリン酸デシル、ラウリン酸ヘキシル、ミリスチン酸デシル、ミリスチン酸ミリスチル、ミリスチン酸セチル、ステアリン酸ステアリル、オレイン酸デシル、リシノレイン酸セチル、ラウリン酸イソステアリル、ミリスチン酸イソトリデシル、ステアリン酸オクチル、ステアリン酸イソセチル、オレイン酸イソデシル、イソステアリン酸イソプロピル、2‐エチルヘキサン酸セトステアリル、2‐エチルヘキサン酸ステアリル、イソステアリン酸ヘキシル、トリカプリル酸グリセリル、トリウンデシル酸グリセリル、トリイソパルミチン酸グリセリル、トリイソステアリン酸グリセリル、オクタン酸イソステアリル、イソノナン酸オクチル、ネオデカン酸ヘキシルデシル、ネオデカン酸オクチルドデシル、イソステアリン酸イソステアリル、およびイソステアリン酸オクチルドデシルなどが挙げられる。また、高級アルコール類として、ラウリルアルコール、オレイルアルコールおよびイソステアリルアルコールなどが挙げられ、脂肪酸類として、オレイン酸およびイソステアリン酸などが挙げられる。また、植物油類として、オリーブ油、大豆油およびホホバ油などが挙げられ、シリコーン油類として、メチルポリシロキサン、メチルフェニルポリシロキサンおよびメチルシクロポリシロキサンなどが挙げられる。   Specific examples of such liquid oily substances include hydrocarbons such as liquid paraffin, α-olefin oligomer and squalane. Examples of ethers include dioctyl ether, ethylene glycol monolauryl ether, ethylene glycol dioctyl ether and glycerol monooleyl ether, and examples of esters include glyceryl tri-2-ethylhexanoate, cetyl 2-ethylhexanoate, isononanoic acid. Isononyl, isotridecyl isononanoate, isopropyl myristate, butyl myristate, octyldodecyl myristate, isopropyl palmitate, ethyl stearate, octyl palmitate, isocetyl isostearate, butyl stearate, ethyl linoleate, isopropyl linoleate, ethyl oleate , Isocetyl myristate, isostearyl myristate, isostearyl palmitate, cetyl palmitate, trimethylolpropane triisostearate, pentaerythritol tetra-2-ethylhexanoate, cetyl caprylate, decyl laurate, hexyl laurate, decyl myristate , Myristyl myristate, cetyl myristate, stearyl stearate, decyl oleate, cetyl ricinoleate, isostearyl laurate, isotridecyl myristate, octyl stearate, isocetyl stearate, isodecyl oleate, isopropyl isostearate, 2-ethylhexane Acid cetostearyl, 2-ethylhexanoic acid stearyl, hexyl isostearate, glyceryl tricaprylate, glyceryl triundecylate, glyceryl triisopalmitate, glyceryl triisostearate, isostearyl octanoate, octyl isononanoate, hexyldecyl neodecanoate, neodecanoic acid Examples include octyldodecyl, isostearyl isostearate, and octyldodecyl isostearate. Examples of higher alcohols include lauryl alcohol, oleyl alcohol and isostearyl alcohol, and examples of fatty acids include oleic acid and isostearic acid. Examples of vegetable oils include olive oil, soybean oil and jojoba oil, and examples of silicone oils include methylpolysiloxane, methylphenylpolysiloxane and methylcyclopolysiloxane.

この発明における液状油性物質(B)は、炭化水素油が占める割合が60質量%以上(60〜100質量%)である。
炭化水素油は、炭素と水素からなる周知の液状化合物であり、通常の化粧料に配合される皮膚に無害なものを適用できる。
炭化水素油の配合量が60質量%未満では、スクラブが崩壊しやすくなったり、平均粒子径0.2mm未満またはそれより極端に小さなスクラブが生成されることになり、外水相が白濁したり、炭化水素油以外の油剤に由来するべたつきが強く使用感が損なわれやすくなる等、化粧料の優れた製品美観と優れた使用感の確実な両立が難しくなるからである。
In the liquid oily substance (B) in the present invention, the proportion of the hydrocarbon oil is 60% by mass or more (60 to 100% by mass).
Hydrocarbon oil is a well-known liquid compound composed of carbon and hydrogen, and can be applied to those that are harmless to the skin, which are usually added to cosmetics.
If the blending amount of the hydrocarbon oil is less than 60% by mass, the scrub tends to disintegrate, scrubs having an average particle size of less than 0.2 mm or extremely smaller than that are generated, and the outer water phase becomes cloudy. The reason is that it is difficult to reliably achieve both excellent product aesthetics and excellent usability of cosmetics, such as strong stickiness derived from an oil agent other than a hydrocarbon oil and easy deterioration of usability.

この発明における固形油性物質(C)は、ヒトの皮膚に接する時に固体であるように、例えば40℃以下で固体であり、化粧料に配合可能な融点40℃以上の皮膚に無害なロウ類、脂肪酸類、高級アルコール類、エーテル類、エステル類などを好適に用いることができる。   The solid oily substance (C) in the present invention is a wax which is solid at, for example, 40 ° C. or lower and is harmless to the skin and has a melting point of 40 ° C. or higher which can be blended into cosmetics, so that it is solid when it comes into contact with human skin. Fatty acids, higher alcohols, ethers, esters and the like can be preferably used.

上記固形油性物質の具体例としては、ロウ類として、カルナウバロウ、キャンデリラロウ、コメヌカロウ、ラノリン、ミツロウなどが挙げられ、脂肪酸類として、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、ベヘニン酸、ヒドロキシステアリン酸などが挙げられる。また高級アルコール類として、セタノール、ステアリルアルコール、ベヘニルアルコール、水添ナタネ油アルコール、アラキルアルコールなどが挙げられ、エーテル類として、バチルアルコール、キミルアルコールなどが挙げられ、さらにまたエステル類として、ミリスチン酸ミリスチル、ミリスチン酸セチル、パルミチン酸セチル、ステアリン酸ステアリル、テトラミリスチン酸ペンタエリスリトール、乳酸セチル、ステアリン酸コレステリル等が挙げられる。   Specific examples of the solid oily substance include waxes such as carnauba wax, candelilla wax, rice bran wax, lanolin and beeswax, and fatty acids as lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, hydroxy. Examples thereof include stearic acid. Further, higher alcohols include cetanol, stearyl alcohol, behenyl alcohol, hydrogenated rapeseed oil alcohol, aralkyl alcohol, and the like, ethers include batyl alcohol, chimyl alcohol, and the like, and as esters, myristic acid Examples thereof include myristyl, cetyl myristate, cetyl palmitate, stearyl stearate, pentaerythritol tetramyristate, cetyl lactate, and cholesteryl stearate.

また、この発明の液状化粧料には、必要に応じて界面活性剤を添加してもよく、例えばポリオキシエチレンベヘニルエーテル、モノステアリン酸ポリエチレングリコール、ポリオキシエチレンセチルエーテル、モノステアリン酸ポリグリセリル、モノステアリン酸ソルビタン、モノラウリン酸ポリグリセリル、ジイソステアリン酸ポリグリセリル、ジステアリン酸ポリグリセリル、ラウロイルグルタミン酸ナトリウム、ベヘントリモニウムクロリド、ステアラミドプロピルジメチルアミン等を添加してもよい。   Further, the liquid cosmetic of the present invention may be added with a surfactant if necessary, for example, polyoxyethylene behenyl ether, polyethylene glycol monostearate, polyoxyethylene cetyl ether, polyglyceryl monostearate, mono Sorbitan stearate, polyglyceryl monolaurate, polyglyceryl diisostearate, polyglyceryl distearate, sodium lauroyl glutamate, behentrimonium chloride, stearamidopropyldimethylamine and the like may be added.

この発明における固形油性物質(C)は、高級アルコール類が占める割合が60質量%以上(60〜100質量%)である。上記高級アルコールは、一般式R−OH(R:脂肪族残基)で表される化合物のうち炭素数が14以上のものであり、通常の化粧料に配合される皮膚に無害なものを好適に用いることができる。因みに、炭素数14の高級アルコールの融点は約38℃である。   The proportion of higher alcohols in the solid oily substance (C) in the present invention is 60% by mass or more (60 to 100% by mass). Among the compounds represented by the general formula R-OH (R: aliphatic residue), the higher alcohols have 14 or more carbon atoms, and those which are harmless to the skin and are usually added to cosmetics are preferred. Can be used for. Incidentally, the melting point of the higher alcohol having 14 carbon atoms is about 38 ° C.

この発明における固形油性物質の配合量が60質量%未満では、スクラブが崩壊しやすくなったり、逆にスクラブが粘着質になる等するため、使用時や輸送時の振動で崩壊や粘着凝集したり、高級アルコール以外の油剤に由来するべたつきが強く使用感が損なわれたりして、化粧料の優れた製品美観と優れた使用感の確実な両立が難しくなるからである。   If the blending amount of the solid oily substance in the present invention is less than 60% by mass, the scrub tends to collapse, or conversely, the scrub becomes sticky, so that it collapses or adheres and agglomerates due to vibration during use or transportation. This is because the stickiness derived from an oil agent other than the higher alcohol is strong and the usability is impaired, and it is difficult to surely achieve both good cosmetic aesthetics and excellent usability.

また、この発明における混合物(A)の液状油性物質(B)と固形油性物質(C)の配合割合は、質量比で(B):(C)=1:(0.05〜10)の範囲である。
なぜなら、液状油性物質(B)に対する固形油性物質(C)の質量比(B):(C)が1:0.05未満では、油性スクラブ粒子の融点が低くなり、製造後に液状のままで合一しやすくなるからであり、また前記質量比が1:10を超えると、油性スクラブ粒子の融点が高くなり、使用時に体温でスクラブが溶けずに体感できる固形物として皮膚上に残り使用感を損なうなど、化粧料の優れた製品美観と優れた使用感の両立を確実に維持することが難しいからである。
Further, the mixing ratio of the liquid oily substance (B) and the solid oily substance (C) of the mixture (A) in the present invention is in the range of (B) :( C) = 1: (0.05-10) by mass ratio. Is.
This is because when the mass ratio (B) :( C) of the solid oily substance (C) to the liquid oily substance (B) is less than 1: 0.05, the melting point of the oily scrub particles becomes low, and the liquid scrub particles remain in a liquid state after being produced. If the mass ratio exceeds 1:10, the melting point of the oily scrub particles will be high, and the scrub will remain on the skin as a solid substance that the scrub will not melt at body temperature during use, resulting in a feeling of use. This is because it is difficult to surely maintain both good cosmetic aesthetics and good usability such as damage.

また、この発明において調整する化粧料は、油性スクラブ粒子の総配合量が化粧料中に0.3〜5.0質量%となることが好ましい。なぜなら、0.3質量%未満の配合量では、使用時のエモリエント感が足らず、目的とする使用感を満足させられず、5.0質量%を超える配合量では、べたつきが強く、目的とする使用感を満足させられないことや、スクラブが多すぎて適切な分散ができずに製品美観を損なうなどにより、化粧料の優れた製品美観と優れた使用感の両立を確実に維持することが難しいからである。   Further, in the cosmetic material to be adjusted in the present invention, it is preferable that the total amount of the oily scrub particles is 0.3 to 5.0 mass% in the cosmetic material. Because, if the blending amount is less than 0.3% by mass, the emollient feeling at the time of use is not sufficient and the desired usability is not satisfied, and if the blending amount is more than 5.0% by mass, the stickiness is strong and it is intended. It is not possible to satisfy the feeling of use, and because the scrub is too much to disperse properly, and the product aesthetics is impaired, it is possible to ensure that both the excellent product aesthetics of cosmetics and the excellent usability are maintained. Because it is difficult.

さらにまた、この発明において調整する化粧料は、外水相に分散している油性スクラブ粒子の平均粒子径が0.2〜2.0mmであることが好ましい。なぜなら、0.2mm未満の小さな平均粒子経では、極端に小さいスクラブが生成されやすくなって外水相に濁りが生じやすくなり、また2.0mmを超える大きな平均粒子経では、使用時にスクラブがなかなか体温で溶解せずに使用感を損ねたり、製造時の粒子径調節が難しくて製造効率が低下するからである。   Furthermore, in the cosmetic material to be adjusted in the present invention, it is preferable that the average particle diameter of the oily scrub particles dispersed in the outer water phase is 0.2 to 2.0 mm. Because, when the average particle size is less than 0.2 mm, extremely small scrubs are likely to be generated and the outer water phase tends to be turbid, and when the average particle size is greater than 2.0 mm, the scrub is difficult to use. This is because it does not melt at body temperature, impairing the feeling of use, and it is difficult to control the particle size during production, resulting in reduced production efficiency.

さらに、この発明において調整する化粧料は、一般的に化粧料製造に使用される機器を用いて製造できるが、攪拌工程では、混合機、分散機、混練機、ホモミキサー、圧力式ホモジナイザーまたは高速攪拌機、より具体的には複合型攪拌機や薄膜旋回型高速ミキサーなどを用いて油性スクラブ粒子と水相を混合することで、油性スクラブ粒子の粒子径を均一化することが好ましい。   Furthermore, the cosmetics to be adjusted in the present invention can be produced by using an apparatus generally used for producing cosmetics, but in the stirring step, a mixer, a disperser, a kneader, a homomixer, a pressure homogenizer or a high speed mixer. It is preferable to make the particle diameter of the oily scrub particles uniform by mixing the oily scrub particles and the aqueous phase using a stirrer, more specifically, a composite stirrer, a thin film swirl type high speed mixer, or the like.

例えば薄膜旋回型高速ミキサーは、高速で旋回する筒形容器内壁面に遠心力で薄膜状の液層を形成し、その内部で攪拌、混合、分散が行われるものであって、例えば旋回する容器内壁面の液層の周速を0.5〜5.0m/s、薄膜内での攪拌混合に要する滞留時間を15〜60秒で行なうことにより、平均粒子径0.8mm程度で粒度分布の範囲が狭く粒子径のばらつきの小さい油性スクラブ粒子群を形成できる。   For example, a thin film swirl type high speed mixer is one in which a thin film liquid layer is formed on the inner wall surface of a cylindrical container that swirls at high speed by centrifugal force, and stirring, mixing and dispersion are performed therein. The peripheral velocity of the liquid layer on the inner wall surface is 0.5 to 5.0 m / s, and the residence time required for stirring and mixing in the thin film is 15 to 60 seconds. It is possible to form a group of oily scrub particles having a narrow range and a small variation in particle size.

このような攪拌・混合・分散は、市販の薄膜旋回型高速ミキサー(プライミクス社製:フィルミックス)を用いて達成することができ、油性スクラブ粒子の粒子径を均一化すると、液状化粧料の製品美観がより優れたものになるだけでなく、品質が安定して使用感のばらつきも少なくなる。   Such stirring / mixing / dispersion can be achieved by using a commercially available thin film swirl type high-speed mixer (Filmix manufactured by Primix Co., Ltd.), and if the particle size of the oily scrub particles is made uniform, a liquid cosmetic product is obtained. Not only does it have a better appearance, but the quality is stable and the usability is reduced.

油性スクラブ粒子の粒子径の均一化は、油性スクラブ粒子の平均粒子径が0.2〜2.0mmである場合に、粒子径のばらつき(標準偏差)を0.10〜0.20mmの範囲(後述する実施例15、16ではそれぞれ0.18mm、0.13mm)として所期した効果が得られている。   The uniformization of the particle diameter of the oily scrub particles is performed by adjusting the variation (standard deviation) of the particle diameters in the range of 0.10 to 0.20 mm when the average particle diameter of the oily scrub particles is 0.2 to 2.0 mm ( In Examples 15 and 16 described later, the intended effect of 0.18 mm and 0.13 mm) is obtained.

この発明において調整される化粧料の外水相の成分は特に限定されないが、配合する化粧料によって適宜選択する方が好ましい。また、この発明の化粧料の調整方法は、特に限定されず、配合する化粧料に対応させて適宜選択することができる。   The components of the external water phase of the cosmetics prepared in the present invention are not particularly limited, but it is preferable to select them appropriately depending on the cosmetics to be blended. The method for adjusting the cosmetic of the present invention is not particularly limited, and can be appropriately selected according to the cosmetic to be blended.

〔実施例1〜3、比較例1〜4〕
表1に示す(B)成分および(C)成分を混合し、その混合物を60〜80℃に加熱して溶解し、次いで前記溶解した60〜80℃の範囲内の温度に加熱した(B)(C)成分以外の成分からなる水相に液状の前記混合物を投入し、攪拌機(東京理化器械社製:マゼラNZ−1100)を用いて回転数100〜500rpmで撹拌しながら冷却することで、平均粒子径が約0.8mmの油性スクラブ粒子を均一に分散させた化粧水を調製した。
得られた化粧水について、以下の評価方法で製造直後及び振動試験後の製品美観並びに使用感を判定した。
[Examples 1 to 3, Comparative Examples 1 to 4]
The components (B) and (C) shown in Table 1 were mixed, and the mixture was heated to 60 to 80 ° C to dissolve it, and then heated to a temperature within the range of the dissolved 60 to 80 ° C (B). By adding the liquid mixture to an aqueous phase consisting of components other than the component (C) and cooling with stirring at a rotation speed of 100 to 500 rpm using a stirrer (Tokyo Rika Kikai Co., Ltd .: Magella NZ-1100), A lotion was prepared by uniformly dispersing oily scrub particles having an average particle diameter of about 0.8 mm.
With respect to the obtained lotion, the product aesthetics and the feeling of use immediately after the production and after the vibration test were judged by the following evaluation methods.

〔評価方法〕(製品美観-製造直後)
製造直後の化粧水を透明容器(竹本容器社製:OPT−100)に充填して静置し、油滴の粒径や形、色などを目視にて観察した。
(Evaluation method) (Product aesthetics-immediately after production)
Immediately after production, the lotion was filled in a transparent container (manufactured by Takemoto Container Co., Ltd .: OPT-100) and allowed to stand still, and the particle size, shape, color, etc. of the oil droplets were visually observed.

[判定]
◎:大変優れた製品美観を有する。(油滴の粒径や形が適切かつ均一で、適切に分散している)
○:優れた製品美観を有する。(油滴の粒径や形にわずかにばらつきがある)
△:好ましくない製品美観を有する。(油滴の粒径や形が不適切であり、分散できていない油相が残存している)
×:大変好ましくない製品美観を有する。(油相が分散していない)
[Judgment]
⊚: The product has a very good appearance. (The size and shape of the oil droplets are appropriate, uniform, and properly dispersed)
◯: The product has an excellent appearance. (Slight variations in particle size and shape of oil droplets)
B: Poor product appearance. (The particle size and shape of the oil droplets are inadequate, and the oil phase that cannot be dispersed remains.)
X: Very unfavorable product appearance. (Oil phase is not dispersed)

〔評価方法〕(製品美観-振動試験後)
得られた化粧水を透明容器に充填し、油滴の粒径や形、色などを目視にて観察した後、容器を振動させ、振動後の油滴の粒径や形、色などを目視で比較観察した。容器の振動は、温度23〜27℃、湿度40〜60%環境下において、容器を180度転倒後に元に戻す操作を30回繰り返すことにより行なった。
(Evaluation method) (Product aesthetics-after vibration test)
After filling the resulting lotion into a transparent container and visually observing the particle size, shape, color, etc. of the oil drops, vibrate the container and visually check the particle size, shape, color, etc. of the oil drops after vibration. Comparative observation was carried out. Vibration of the container was carried out by repeating the operation of returning the container to its original position after inclining 180 degrees repeatedly 30 times in an environment of a temperature of 23 to 27 ° C. and a humidity of 40 to 60%.

[判定]
◎:振動後も製品美観が全く損なわれない。(振動後も製品外観が変化しない)
○:振動後も製品美観がほとんど損なわれない。(振動により油滴が若干小さくなったり、水相が若干白濁する)
△:振動後は製品外観が損なわれる。(振動により油滴が非常に小さくなり、水相が白濁する)
×:振動後は製品外観を完全に損なわれる。(振動により油滴が見えなくなり、均一で白濁な外観となる)
[Judgment]
⊚: Product aesthetics are not impaired even after vibration. (Product appearance does not change after vibration)
◯: Product aesthetics are hardly impaired even after vibration. (Oil drops become slightly smaller due to vibration, or the water phase becomes slightly cloudy)
Δ: The product appearance is impaired after vibration. (Oil drops become very small due to vibration, and the water phase becomes cloudy)
X: The appearance of the product is completely impaired after vibration. (Oil drops disappear due to vibration, resulting in a uniform and cloudy appearance)

〔評価方法〕(使用感)
評価パネル20名(20歳代〜40歳代の成人男女各10名)により、皮膚に塗布した際の使用感(べたつき感など)を下記基準にて5段階評価し、さらにその平均点から判定した。
[Evaluation method] (Usage)
Evaluation panel 20 people (10 adults and 10 people each in their 20s to 40s) evaluated the feeling of use (stickiness etc.) when applied to the skin in 5 levels according to the following criteria, and judged from the average score. did.

[評価]
5点:非常に良い。
4点:良い。
3点:普通。
2点:悪い。
1点:非常に悪い。
[Evaluation]
5 points: Very good.
4 points: Good.
3 points: Normal.
2 points: Bad.
1 point: Very bad.

[判定]
◎:平均点4点以上
○:平均点3点以上4点未満
△:平均点2点以上3点未満
×:平均点2点未満
[Judgment]
◎: Average score of 4 points or more ○: Average score of 3 points or more and less than 4 points △: Average score of 2 points or more and less than 3 points ×: Average point of less than 2 points

表1に示される結果からも明らかなように、実施例1、2では、液状油性物質(B)として炭化水素油を用いているため、優れた製品美観および使用感を有する化粧水が得られた。   As is clear from the results shown in Table 1, in Examples 1 and 2, since the hydrocarbon oil was used as the liquid oily substance (B), lotions having excellent product aesthetics and feeling of use were obtained. It was

一方、比較例1、2では、液状油性物質(B’)としてエステル油や脂肪酸を用いており、そのために粒子が崩れやすくなり、撹拌工程により粒子が必要以上に微細化された化粧水が得られた。これらは、振動試験により、粒子がさらに微細化されたため、製品美観を保つことができなかった。   On the other hand, in Comparative Examples 1 and 2, ester oils and fatty acids are used as the liquid oily substance (B ′), so that the particles are easily broken and the lotion is obtained by the stirring step in which the particles are made finer than necessary. Was given. These products were unable to maintain the product aesthetics because the particles were further miniaturized by the vibration test.

また、比較例3は、液状油性物質(B’)としてシリコーン油を用いており、固形油性物質(C)との相溶性が悪かったため、製造工程中に液状油性物質(B’)と固形油性物質(C)が分離し、均一な球状の油性スクラブ粒子を形成することができなかった。また、得られた化粧水を透明容器に充填すると、シリコーン油は容器壁面に付着し、使用に際してシリコーン油を容器から取り出すことが困難であった。   In Comparative Example 3, silicone oil was used as the liquid oily substance (B ′), and the compatibility with the solid oily substance (C) was poor, so that the liquid oily substance (B ′) and the solid oily substance were not mixed during the production process. The substance (C) was separated, and uniform spherical oily scrub particles could not be formed. Further, when the obtained lotion was filled in a transparent container, the silicone oil adhered to the wall surface of the container, and it was difficult to take out the silicone oil from the container during use.

また、比較例4は、実施例1と比較例1の中間の組成により得られた化粧水であり、比較例1と同様に粒子が微細化されやすく、優れた製品美観を有していなかった。
比較例4から液状油性物質(B)中の炭化水素油比率をさらに高めた実施例3の化粧水は、粒子がある程度微細化され難くなり、振動試験で製品仕様が損なわれなかった。
Further, Comparative Example 4 is a lotion obtained by the composition intermediate between Example 1 and Comparative Example 1, and like the Comparative Example 1, the particles were easily finely divided and did not have an excellent product aesthetics. ..
In the lotion of Example 3 in which the ratio of hydrocarbon oil in the liquid oily substance (B) was further increased from Comparative Example 4, the particles were difficult to be refined to some extent, and the product specifications were not impaired in the vibration test.

〔実施例4〜5、比較例5〜9〕
表2に示す組成の成分を用いること以外は、実施例1と全く同様にして化粧水を調製し、前記及び以下に記載する評価方法を用いて、製造直後及び振動試験後の製品美観、使用感並びに平均粒子径について判定した。また、製造直後の実施例4、実施例5、比較例6、及び比較例7の製品美観については、それぞれ化粧水を充填した透明容器の写真を図1または図2に示した。
[Examples 4-5, Comparative Examples 5-9]
A lotion was prepared in exactly the same manner as in Example 1 except that the components having the composition shown in Table 2 were used, and the cosmetic appearance and use immediately after production and after vibration test were performed using the evaluation methods described above and below. The feeling and average particle size were evaluated. Regarding the product aesthetics of Example 4, Example 5, Comparative Example 6, and Comparative Example 7 immediately after production, photographs of transparent containers filled with lotion are shown in FIG. 1 or FIG.

〔評価方法〕(平均粒子径)
得られた化粧料をマイクロスコープ(VHX-6000(株式会社キーエンス製))で観察し、得られた画像を内蔵システム(メイン計測システム)にて処理することにより平均粒子径を算出した。
(Evaluation method) (Average particle size)
The obtained cosmetics were observed with a microscope (VHX-6000 (manufactured by Keyence Corporation)), and the obtained images were processed by a built-in system (main measurement system) to calculate the average particle size.

表2に示される結果からも明らかなように、実施例4の化粧水は、固形油性物質(C)として炭素数22のベヘニルアルコールを用いており、優れた製品美観及び使用感を有していた。すなわち、図1の写真の左側に示される透明容器に充填された実施例4の化粧水は、油滴が適切な大きさで均一に分散し、外水相も透明で美しい美観を呈していた。   As is clear from the results shown in Table 2, the lotion of Example 4 used behenyl alcohol having 22 carbon atoms as the solid oily substance (C), and had an excellent product aesthetics and feeling of use. .. That is, in the lotion of Example 4 filled in the transparent container shown on the left side of the photograph in FIG. 1, oil droplets were dispersed uniformly in an appropriate size, and the external water phase was also transparent and had a beautiful appearance. ..

一方、比較例5の化粧水は、固形油性物質(C’)としてロウ類を用いたものであり、粒子にロウ類特有の粘りが付与され、製造工程中や振動試験において粒子同士が接着して製品美観が損なわれ、また使用感においてもべたつきが非常に強く認められた。   On the other hand, the lotion of Comparative Example 5 uses waxes as the solid oily substance (C ′), and the particles have a stickiness peculiar to waxes, and the particles adhere to each other during the manufacturing process or in the vibration test. As a result, the aesthetics of the product was impaired, and the product was extremely sticky in the feeling of use.

また、比較例6−8では、固形油性物質(C’)として、それぞれ脂肪酸、エステル油、親水性界面活性剤を単独で用いたところ、炭素数14以上の高級アルコールが所定量含まれていないため、粒子が崩れやすくなり、製造工程や振動試験において粒子が微細化されやすく、所期した粒径の油性スクラブ粒子が分散せず、製品美観の好ましい化粧水は得られなかった。   Further, in Comparative Examples 6-8, when a fatty acid, an ester oil, and a hydrophilic surfactant were used alone as the solid oily substance (C ′), respectively, a predetermined amount of higher alcohol having 14 or more carbon atoms was not contained. Therefore, the particles are likely to be broken, the particles are easily miniaturized in the manufacturing process or the vibration test, the oily scrub particles having a desired particle size are not dispersed, and a lotion having a good product appearance cannot be obtained.

図2の写真に示される透明容器に充填された比較例6(同写真左側)及び比較例7(同写真右側)の化粧水は、油性スクラブの粒子径が小さすぎ、また粒子径が小さくなり過ぎた影響で化粧水全体が白濁し、製品美観が損なわれていた。
また、比較例9は、実施例4と比較例6の中間の組成により得られた化粧水であるが、比較例6と同様に粒子が微細化されやすいものであり、透明性のある所期した製品美観を呈しなかった。
The lotions of Comparative Example 6 (left side of the same photograph) and Comparative Example 7 (right side of the same photograph) filled in the transparent container shown in the photograph of FIG. 2 have an oily scrub having a too small particle size and a small particle size. Due to the excess, the whole lotion became cloudy and the product aesthetics was impaired.
Further, Comparative Example 9 is a lotion obtained with a composition intermediate between Example 4 and Comparative Example 6, but like the Comparative Example 6, the particles are likely to be finely divided and are expected to have transparency. The product did not have the aesthetic appeal.

また、実施例5は、比較例9から固形油性物質(C)の含有する炭素数14以上の高級アルコール比率を高めたものであり、粒子がある程度微細化され難く、振動試験でも製品美観の損なわれない化粧水であった。すなわち、図1の写真の右側に示される透明容器に充填された実施例5の化粧水は、油滴が適切な大きさで均一に分散し、外水相も透明で美しい美観を呈していた。   Further, in Example 5, the ratio of the higher alcohol having a carbon number of 14 or more contained in the solid oily substance (C) is increased from that of Comparative Example 9, the particles are difficult to be refined to some extent, and the appearance of the product is impaired even in the vibration test. It was a lotion. That is, in the lotion of Example 5 filled in the transparent container shown on the right side of the photograph in FIG. 1, oil droplets were dispersed uniformly in an appropriate size, and the external water phase was also transparent and had a beautiful appearance. ..

〔実施例6〜10、比較例10〜11〕
表3に示す組成の成分を用いること以外は、実施例1と全く同様にして化粧水を調製し、前記した評価方法を用いて、製造直後及び振動試験後の製品美観並びに使用感について判定した。
[Examples 6 to 10 and Comparative Examples 10 to 11]
A lotion was prepared in exactly the same manner as in Example 1 except that the components having the compositions shown in Table 3 were used, and the aesthetics of the product immediately after the production and after the vibration test and the feeling of use were determined using the above-described evaluation method. ..

表3に示される結果からも明らかなように、実施例7−9は、液状油性物質(B)と固形油性物質(C)の質量比が、1:(0.10〜5.0)の範囲内の混合物からなる油性スクラブ粒子が分散し、優れた製品美観及び使用感を有する化粧水が得られた。   As is clear from the results shown in Table 3, in Examples 7-9, the mass ratio of the liquid oily substance (B) and the solid oily substance (C) was 1: (0.10 to 5.0). Oily scrub particles consisting of a mixture within the range were dispersed, and a lotion having excellent product aesthetics and feeling of use was obtained.

また、上記質量比が1:0.05となる実施例6の化粧水では、固形油の硬さが粒子に付与されにくいために振動試験により粒子が僅かに微細化されたが、使用感に問題はなかった。
また、実施例6からさらに固形油性物質比率を下げた比較例10では、振動試験での粒子微細化が顕著となり、製品美観を保つことができなくなった。
Further, in the lotion of Example 6 in which the mass ratio was 1: 0.05, the hardness of the solid oil was not easily imparted to the particles, so the particles were slightly fined by the vibration test. There was no problem.
Further, in Comparative Example 10 in which the solid oily substance ratio was further reduced from that in Example 6, the grain refinement in the vibration test became remarkable, and the product aesthetics could not be maintained.

上記質量比が1:10となる実施例10の化粧水は、油性スクラブ粒子の融点が高くなり、塗布時に溶解するまでに時間が長くなったが、使用に耐えるものであった。
実施例10からさらに固形油性物質(C)の比率を上げた比較例11は、使用時に粒子が溶解せず使用感が損なわれ、また通常の製造温度では撹拌分散工程中に油性スクラブ粒子が一部固化してしまい、好ましくない美観を呈する化粧水となった。
In the lotion of Example 10 in which the mass ratio was 1:10, the melting point of the oily scrub particles was high, and it took a long time to dissolve at the time of application, but it was usable.
In Comparative Example 11 in which the ratio of the solid oily substance (C) was further increased from Example 10, the particles did not dissolve during use and the feeling of use was impaired, and at normal manufacturing temperatures, oily scrub particles were less likely to be present during the stirring and dispersing process. The part solidified and became a lotion with an unpleasant aesthetic appearance.

〔実施例1、11〜14、比較例12〜13〕
表4に示す組成の成分を用いること以外は、実施例1と全く同様にして化粧水を調製し、前記した評価方法を用いて、製造直後及び振動試験後の製品美観並びに使用感について判定した。なお、参考のために実施例1も同表中に併記した。
[Examples 1, 11 to 14, Comparative Examples 12 to 13]
A lotion was prepared in exactly the same manner as in Example 1 except that the components having the compositions shown in Table 4 were used, and the aesthetics of the product immediately after the production and after the vibration test and the feeling of use were determined using the above-described evaluation method. .. For reference, Example 1 is also shown in the table.

表4に示される結果からも明らかなように、油性スクラブ粒子の含有量として[(B)+(C)]が化粧料100質量%中に0.5〜1.0質量%配合された実施例12、13、実施例1の化粧水は、優れた製品美観及び使用感を有していた。   As is clear from the results shown in Table 4, as the content of the oily scrub particles, [(B) + (C)] was blended in an amount of 0.5 to 1.0% by mass in 100% by mass of the cosmetic material. The lotions of Examples 12, 13 and Example 1 had excellent product aesthetics and feeling of use.

油性スクラブ粒子の配合割合を0.3質量%とした実施例11の化粧水は、油性物質によるべたつき感が僅かに弱い使用感であった。
油性スクラブ粒子の配合割合が実施例11より少ない比較例12は、油性物質によるべたつき感がほとんど感じられず、あまり好ましくない使用感であった。
The lotion of Example 11 in which the mixing ratio of the oily scrub particles was 0.3% by mass had a slightly weak feeling of use due to the oily substance.
In Comparative Example 12 in which the mixing ratio of the oily scrub particles was smaller than that in Example 11, almost no sticky feeling due to the oily substance was felt, and the use feeling was not so preferable.

油性スクラブ粒子の配合割合が5.0質量%の実施例14は、油性物質によるべたつき感が適度にある使用感であり、また化粧水中の油滴の密度が高くなり、製品美観も良い化粧水であった。
油性スクラブ粒子の配合割合を実施例14より増加させた比較例13は、油性物質によるべたつき感が強くなり過ぎて使用感が損なわれ、また適切に油滴を分散させることができなかった。
Example 14 in which the mixing ratio of the oily scrub particles is 5.0% by mass has a feeling of use with an appropriate greasy feel due to the oily substance, and the density of oil droplets in the lotion is high, and the lotion has a good product appearance. Met.
In Comparative Example 13 in which the mixing ratio of the oily scrub particles was increased from that in Example 14, the sticky feeling due to the oily substance became too strong, the use feeling was impaired, and the oil droplets could not be dispersed appropriately.

〔実施例15〜16〕
実施例15は、表5に示す成分を用いたこと以外は実施例1と全く同様にして化粧水を調製し、実施例16は、表5に示す成分を用いたこと及び高速攪拌機として薄膜旋回型高速ミキサー(プライミクス社製:フィルミックス)を用いて周速0.5〜1.0m/s、攪拌機内の滞留時間20〜30秒の製造条件としたこと以外は実施例1と全く同様にして、各実施例についてサンプル数9個(ロット単位3個の3ロット)の化粧水を調製した。
[Examples 15 to 16]
In Example 15, a lotion was prepared in exactly the same manner as in Example 1 except that the components shown in Table 5 were used. In Example 16, the components shown in Table 5 were used and the thin film swirling was performed as a high-speed stirrer. Example 1 exactly the same as in Example 1 except that the peripheral speed was 0.5 to 1.0 m / s and the residence time in the stirrer was 20 to 30 seconds using a mold high-speed mixer (Filmix). As a result, a lotion containing 9 samples (3 lots of 3 lots) was prepared for each example.

そして、前記および以下に記載する評価方法を用いて、製造直後及び振動試験後の製品美観、使用感を調べ、実施例4と同様にして平均粒子径、並びに以下の評価方法で粒子径のばらつきを評価し判定した。また、実施例15、16の化粧水中の油性スクラブ粒子の形態を示す顕微鏡写真を図3、図4に示した。   Then, using the evaluation methods described above and below, the product aesthetics and the feeling of use immediately after the production and after the vibration test were examined, and the average particle diameter was measured in the same manner as in Example 4, and the dispersion of the particle diameters was evaluated by the following evaluation methods. Was evaluated and judged. Further, micrographs showing the morphology of the oily scrub particles in the lotion of Examples 15 and 16 are shown in FIGS. 3 and 4.

〔評価方法〕(粒子径のばらつき)
同一組成で3ロット製造して得られたた化粧水をマイクロスコープ(キーエンス社製:VHX-6000)で観察し、得られた画像を内蔵システム(メイン計測システム)にて処理することにより平均粒子径およびそのばらつきとして標準偏差を算出した。さらに、評価パネル20名(20歳代〜40歳代の成人男女各10名)により、皮膚に塗布した際の使用感(べたつき感など)を評価することで、ロット間のばらつきを判定した。
[Evaluation method] (Dispersion of particle size)
Average lotion by observing the lotion obtained by manufacturing 3 lots with the same composition with a microscope (VHX-6000 manufactured by Keyence) and processing the obtained image with the built-in system (main measurement system) The standard deviation was calculated as the diameter and its variation. Furthermore, the evaluation panel 20 persons (10 adult males and females in their 20s to 40s each) evaluated the feeling of use (such as sticky feeling) when applied to the skin to determine the variation between lots.

[判定]
◎:ロット間で粒子径および使用感のばらつきがほとんどない。
○:ロット間で粒子径のばらつきがわずかにあるが、使用感への影響はほとんどない。
△:ロット間で粒子径のばらつきが大きく、使用感にも影響する。
×:ロット間で粒子径のばらつきが非常に大きく、使用感も異なる。
[Judgment]
⊚: There is almost no variation in particle size and feeling between lots.
◯: There is slight variation in particle size between lots, but there is almost no effect on usability.
Δ: The particle size varies greatly among lots, which also affects the feeling of use.
X: The particle size varies greatly among lots, and the feeling of use also differs.

表5に示される結果からも明らかなように、攪拌工程で、薄膜旋回型高速ミキサーを使用しない実施例15の化粧水は、平均粒子径は0.46mm、粒子径のばらつき(標準偏差は約0.18mm)はわずかであった。また実施例15の化粧水は、図3の顕微鏡写真からも明らかなように、粒子径のばらつきが大きく、また小さくいびつな形状の粒子が形成されていた。   As is clear from the results shown in Table 5, the lotion of Example 15 in which the thin film swirl type high-speed mixer was not used in the stirring step had an average particle size of 0.46 mm and a variation in particle size (standard deviation was about 0.18 mm) was slight. In addition, as is clear from the micrograph of FIG. 3, the lotion of Example 15 had large variations in particle size and small distorted particles were formed.

薄膜旋回型高速ミキサーを使用した実施例16の化粧水は、平均粒子径が0.47mm、粒子径のばらつき(標準偏差は約0.13mm)は殆どなかった。また実施例16の化粧水は、図4の顕微鏡写真からも明らかなように、粒子径のばらつきが比較的小さく、いびつな形状の粒子の形成は見られなかった。
この発明の実施形態と同様に製造可能な各種化粧料の処方例(組成)を以下の表6にまとめて示した。
The lotion of Example 16 using a thin film swirl type high speed mixer had an average particle diameter of 0.47 mm and almost no variation in particle diameter (standard deviation of about 0.13 mm). Further, as is clear from the micrograph of FIG. 4, the lotion of Example 16 had a relatively small variation in particle size, and formation of distorted particles was not observed.
Formulation examples (compositions) of various cosmetics that can be produced similarly to the embodiment of the present invention are summarized in Table 6 below.

Claims (7)

室温で液体の液状油性物質(B)及び室温で固体の固形油性物質(C)の混合物(A)からなる油性スクラブ粒子が外水相に分散している透明または半透明の液状化粧料において、
前記混合物(A)が、質量比で液状油性物質(B):固形油性物質(C)=1:(0.05〜10)の混合物であり、
前記液状油性物質(B)が、炭化水素油を60質量%以上含有し、
前記固形油性物質(C)が、炭素数14以上の高級アルコールを60質量%以上含有することを特徴とする液状化粧料。
A transparent or translucent liquid cosmetic in which oily scrub particles consisting of a mixture (A) of a liquid oily substance (B) which is liquid at room temperature and a solid oily substance (C) which is solid at room temperature are dispersed in an outer water phase,
The mixture (A) is a mixture of a liquid oily substance (B): solid oily substance (C) = 1: (0.05 to 10) in a mass ratio,
The liquid oily substance (B) contains at least 60 mass% of hydrocarbon oil,
A liquid cosmetic, wherein the solid oily substance (C) contains 60% by mass or more of a higher alcohol having 14 or more carbon atoms.
上記油性スクラブ粒子の液状化粧料100質量%中の含有量が、0.3〜5.0質量%である請求項1に記載の液状化粧料。   The liquid cosmetic according to claim 1, wherein the content of the oily scrub particles in 100% by mass of the liquid cosmetic is 0.3 to 5.0% by mass. 前記油性スクラブ粒子が、平均粒子径0.2〜2.0mmの油性スクラブ粒子である請求項1に記載の液状化粧料。   The liquid cosmetic according to claim 1, wherein the oily scrub particles are oily scrub particles having an average particle diameter of 0.2 to 2.0 mm. 上記炭化水素油が、スクワラン、α‐オレフィンオリゴマー、流動パラフィンから選ばれる1種以上の炭化水素油である請求項1に記載の液状化粧料。   2. The liquid cosmetic according to claim 1, wherein the hydrocarbon oil is one or more kinds of hydrocarbon oil selected from squalane, α-olefin oligomer and liquid paraffin. 上記固形油性物質が、セタノール、ベヘニルアルコール、水添ナタネ油アルコール、ステアリルアルコールから選ばれる1種以上の固形油性物質である請求項1に記載の液状化粧料。   The liquid cosmetic according to claim 1, wherein the solid oily substance is one or more solid oily substances selected from cetanol, behenyl alcohol, hydrogenated rapeseed oil alcohol, and stearyl alcohol. 室温で液体の液状油性物質(B)及び室温で固体の固形油性物質(C)の混合物(A)を60〜80℃に加熱して溶解させ、次いで60〜80℃に加熱した水相に投入し、攪拌して前記混合物(A)を球状化した後、冷却して油性スクラブ粒子が外水相に均一分散した透明または半透明の液状化粧料を得る工程からなり、
前記混合物(A)が、質量比で液状油性物質(B):固形油性物質(C)=1:(0.05〜10)の混合物であり、
前記液状油性物質(B)が、炭化水素油を60質量%以上含有し、
前記固形油性物質(C)が、炭素数14以上の高級アルコールを60質量%以上含有する液状化粧料の製造方法。
A mixture (A) of a liquid oily substance (B) which is liquid at room temperature and a solid oily substance (C) which is solid at room temperature is heated to 60 to 80 ° C. to be dissolved, and then added to an aqueous phase heated to 60 to 80 ° C. Then, the mixture (A) is spheroidized by stirring and then cooled to obtain a transparent or translucent liquid cosmetic in which the oily scrub particles are uniformly dispersed in the outer water phase.
The mixture (A) is a mixture of a liquid oily substance (B): solid oily substance (C) = 1: (0.05 to 10) in a mass ratio,
The liquid oily substance (B) contains 60 mass% or more of hydrocarbon oil,
The method for producing a liquid cosmetic, wherein the solid oily substance (C) contains 60% by mass or more of a higher alcohol having 14 or more carbon atoms.
前記攪拌が、混合機、分散機、混練機、ホモミキサー、圧力式ホモジナイザーまたは高速攪拌機を用いて粒子径を均一化する攪拌である請求項6に記載の液状化粧料の製造方法。   The method for producing a liquid cosmetic according to claim 6, wherein the stirring is stirring for homogenizing the particle diameter using a mixer, a disperser, a kneader, a homomixer, a pressure homogenizer or a high-speed stirrer.
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