WO2019013238A1 - Scrub agent for cosmetics - Google Patents

Scrub agent for cosmetics Download PDF

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Publication number
WO2019013238A1
WO2019013238A1 PCT/JP2018/026125 JP2018026125W WO2019013238A1 WO 2019013238 A1 WO2019013238 A1 WO 2019013238A1 JP 2018026125 W JP2018026125 W JP 2018026125W WO 2019013238 A1 WO2019013238 A1 WO 2019013238A1
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WO
WIPO (PCT)
Prior art keywords
fatty acid
polyhydric alcohol
scrub agent
agent
scrub
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PCT/JP2018/026125
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French (fr)
Japanese (ja)
Inventor
宗一郎 神谷
Original Assignee
理研ビタミン株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by 理研ビタミン株式会社 filed Critical 理研ビタミン株式会社
Priority to JP2019529754A priority Critical patent/JP6990706B2/en
Publication of WO2019013238A1 publication Critical patent/WO2019013238A1/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
    • 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
    • A61K8/37Esters of carboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin

Definitions

  • the present invention relates to a scrub agent used for a cleansing agent, a cleansing agent such as a cleansing agent, a face wash, a hand washing agent, a body cleansing agent, and a cosmetic agent such as a massage agent.
  • a cleansing agent such as a cleansing agent, a face wash, a hand washing agent, a body cleansing agent, and a cosmetic agent such as a massage agent.
  • scrubbing agents have been added to cosmetics such as cleansing agents and massage agents for the purpose of removing dirt from the skin and old keratin and obtaining a massage effect.
  • conventional scrubbing agents particles of synthetic resin (microbeads etc.), particles of calcium carbonate, particles of crushed plant seeds such as walnut and apricot, particles of natural wax such as candelilla wax and carnauba wax, etc. are used. (Patent Documents 1 to 5).
  • An object of the present invention is to provide a cosmetic scrubbing agent comprising a polyhydric alcohol fatty acid ester, which is a chemically synthesized synthetic wax, as a main component.
  • a scrub agent for example, a scrub agent for cosmetics
  • a scrub agent which is a particle containing a polyhydric alcohol fatty acid ester having a median diameter of 50 to 2000 ⁇ m and a melting point of 50 ° C. or higher.
  • [5] A particle containing a polyhydric alcohol fatty acid ester having a median diameter of 50 to 2000 ⁇ m and a melting point of 50 ° C. or more, and particles of 355 ⁇ m or less (eg, about 150 to 355 ⁇ m) Above, 35% or more, 40% or more) containing scrub agent (for example, cosmetic scrub agent).
  • scrub agent for example, cosmetic scrub agent
  • a cosmetic composition comprising the scrub agent according to any one of the above [1] to [5] (for example, a cosmetic scrub agent).
  • a method for cleaning a target site eg, face, body, hands, whole body, etc.
  • a massage method for a target site (eg, face, body, hands, whole body, etc.) using the scrub agent or composition according to any one of the above [1] to [6].
  • a method for cleaning and massaging a target site (eg, face, body, hands, whole body, etc.) using the scrub agent or composition according to any one of the above [1] to [6].
  • the scrub agent for cosmetics of the present invention achieves the same cleaning effect and massage effect as the cosmetic composition using the conventionally used scrub agent (particles of synthetic resin) by being used in the cosmetic composition. be able to.
  • the cosmetic scrub agent of the present invention is mainly composed of polyhydric alcohol fatty acid ester, which is a synthetic wax that can be synthesized chemically, stable supply is possible, and further it is possible to release it in the environment for a long time There is little adverse effect on the environment without remaining over
  • the present invention can also provide a cosmetic scrubbing agent excellent in storage stability.
  • the cosmetic scrub agent of the present invention (hereinafter, also simply referred to as "scrub agent”) is a particle containing a polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more as a main component, and having a median diameter of 50 to 2000 ⁇ m.
  • the polyhydric alcohol fatty acid ester used in the present invention is a substance in which a polyhydric alcohol and a fatty acid are ester-bonded, and is a synthetic wax that can be chemically synthesized.
  • the polyhydric alcohol constituting the polyhydric alcohol fatty acid ester is not particularly limited as long as it is an alcohol containing two or more hydroxyl groups in one molecule, and examples thereof include ethylene glycol, 1,3-propanediol, propylene glycol, 1 , 4-butanediol, 1,2-butanediol, 2-methyl-1,3-propanediol, 1,5-pentanediol, neopentyl glycol, 1,6-hexanediol, 2-ethyl-2-methyl- 1,3-propanediol, 1,7-heptanediol, 2-methyl-2-propyl-1,3-propanediol, 2,2-diethyl-1,3-propanediol, 1,8-octanediol, 1 , 9-nonanediol, 1,10-decanediol, 1,11-undecanedio
  • saccharides and the like which are trivalent or higher polyhydric alcohols such as xylose, arabinose, ribose, rhamnose, glucose, fructose, galactose, mannose, sorbose, cellobiose, maltose, isomaltose, trehalose, sucrose, raffinose, gentianose, melenditose, etc. Can also be mentioned.
  • polyhydric alcohols glycerin, polyglycerin; sorbitol, sorbitan; alkylene glycols such as ethylene glycol and propylene glycol and polymers thereof; pentaerythritol, dipentaerythritol, trimethylolpropane and the like are easily available. It is preferable because it is relatively easy to esterify the polyhydric alcohol and the fatty acid.
  • These polyhydric alcohols may be used alone or in combination of two or more.
  • the fatty acid constituting the polyhydric alcohol fatty acid ester may be a linear fatty acid or a branched fatty acid, and may be any fatty acid of saturated fatty acid or unsaturated fatty acid, but is a fatty acid having 8 to 24 carbon atoms Is preferred.
  • Such fatty acids include, for example, caprylic acid, 2-ethylhexanoic acid, isononanoic acid, capric acid, lauric acid, myristic acid, isomyristic acid, palmitic acid, isopalmic acid, stearic acid, isostearic acid, licinoleic acid, Oleic acid, linoleic acid, linolenic acid, arachidic acid, isoarachidic acid, behenic acid, erucic acid and the like can be mentioned.
  • fatty acids palmitic acid, stearic acid, behenic acid and the like are preferable because when they are polyhydric alcohol fatty acid esters, they exhibit a suitable melting point and a high scrubbing effect.
  • These fatty acids may be used alone or in combination of two or more.
  • the hydroxyl value of the polyhydric alcohol fatty acid ester is not particularly limited, but is preferably 200 mg KOH / g or less, more preferably 100 mg KOH / g or less, still more preferably 80 mg KOH / g or less, and 50 mg KOH / g or less For example, 40 mg KOH / g or less, 30 mg KOH / g or less, 25 mg KOH / g or less, 20 mg KOH / g or less, etc. may be used.
  • a cosmetic composition having excellent storage stability can be efficiently obtained.
  • hydroxyl value of polyhydric-alcohol fatty acid ester can be measured according to the reference
  • the polyhydric alcohol fatty acid ester used in the present invention has a melting point of 50 ° C. or more, preferably 60 ° C. or more. It is preferable that the melting point of the polyhydric alcohol fatty acid ester is 50 ° C. or higher because the hardness is appropriate as a scrub agent at the time of use.
  • the upper limit of the melting point of the polyhydric alcohol fatty acid ester is not particularly limited, but is preferably 100 ° C. or less, more preferably 90 ° C. or less, and still more preferably 80 ° C. or less. When the upper limit of the melting point of the polyhydric alcohol fatty acid ester is below the above, it is preferable because it can be easily processed into the shape of particles.
  • the melting point of polyhydric alcohol fatty acid ester can be measured based on the standard fat and oil analysis method 2.2.4.2-1996 melting point (rising melting point).
  • the polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or higher used in the present invention can be produced by ester bonding a polyhydric alcohol and a fatty acid by a known method, for example, fatty acid and polyhydric alcohol in a reactor. Can be introduced into the reaction mixture and the esterification reaction can be carried out with stirring in the absence of a catalyst or in the presence of a catalyst to produce a polyhydric alcohol fatty acid ester. There is no particular limitation on the temperature of the reaction, but for example, it is preferable to carry out in the temperature range of 150 to 300 ° C.
  • esterification reaction in order to prevent oxidative degradation of polyhydric alcohol fatty acid ester, it is preferable to carry out the esterification reaction while purging the inside of the reactor with nitrogen. After the esterification reaction, if necessary, in order to remove unreacted fatty acid and polyhydric alcohol, distillation under reduced pressure or washing with water after neutralization with alkali may be performed.
  • the scrub agent of the present invention is a solid particle at normal temperature (0 to 30 ° C.) in order to exert a feeling of use as a scrub agent and a cleaning effect.
  • the median diameter of the particles is 50 to 2000 ⁇ m, preferably 100 to 1000 ⁇ m, and more preferably 200 to 500 ⁇ m.
  • the particle size distribution of the scrubbing agent is not particularly limited, but may be appropriately selected depending on the desired physical properties and the like.
  • a scrub agent containing particles of 355 ⁇ m or less eg, about 150 to 355 ⁇ m
  • a scrub agent containing particles of 355 ⁇ m or more eg, 500 ⁇ m or more, 500 ⁇ m or more, 850 ⁇ m or more, 850 ⁇ m or more
  • a scrub agent containing particles of 355 ⁇ m or more eg, 500 ⁇ m or more, 500 ⁇ m or more, 850 ⁇ m or more, 850 ⁇ m or more
  • preferably 10% or more, more preferably 30% or more eg 35% or more, 40% or more
  • the median diameter is an average particle diameter (d50) corresponding to 50% of the integrated distribution curve on a volume basis.
  • the median diameter and the particle size distribution can be measured, for example, by a sonic vibration type fully automatic sieving particle size distribution measuring instrument (model: RPS-85; manufactured by Seishin Co., Ltd.).
  • the scrub agent of the present invention contains polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more as a main component as described above.
  • “main component” means, for example, that 70% by mass or more of polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more is contained in the scrub agent, preferably 80% by mass or more, and more preferably 90% by mass. % Or more, still more preferably 95% by mass or more.
  • the scrub agent of the present invention may contain, in addition to the polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more as the main component, other components in the range not to inhibit the effects of the present invention.
  • Wax, natural wax and the like can be mentioned.
  • the hydrocarbon wax include polyethylene wax, polypropylene wax, microcrystalline wax, paraffin wax, Fischer-Tropsch wax and the like, and carboxylic acid-modified waxes thereof, and natural waxes such as carnauba wax, candelilla wax, rice wax And beeswax, montan wax and the like.
  • the method for producing the scrub agent of the present invention is not particularly limited.
  • a polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or higher and optionally other components are heated to prepare a solution mixture, and then cooled. And solidify and then pulverize and size the particles with a grinder or the like to produce a particulate scrub agent, the above mixture in solution form is directly sprayed in cold air to coagulate the particulate scrub agent.
  • a known method such as a method of producing, a method of producing a particulate scrub agent after spray-drying after adding the above solution mixture and water, an excipient (dextrin, casein sodium etc.), etc. and emulsifying is used. be able to.
  • a scrub agent having a particle diameter is also possible to produce a scrub agent having a particle diameter according to the purpose by granulating, sieving, etc. the obtained particulate scrub agent.
  • the above granulation method is not particularly limited, but, for example, known methods such as stirring granulation method, fluidized bed granulation method, extrusion granulation method, rolling granulation method, compression granulation method and the like can be adopted. .
  • the shape of the scrub agent of the present invention is not particularly limited as long as it is a particle having a median diameter of 50 to 2000 ⁇ m, for example, any of spherical, elliptical, scaly, flake, plate, rod, needle, etc. It may be in the form of Further, the structure of the scrub agent of the present invention is not particularly limited, but may be, for example, a porous structure having a space in the scrub agent considering disintegrability etc., or a dense structure having no space, etc. .
  • the scrubbing agent of the present invention can be used as a commercially available polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more, as it is or by sieving, etc., to a particle diameter according to the purpose.
  • Rikemar TG-12 (trade name; 12-hydroxystearic acid triglyceride manufactured by Riken Vitamin Co., Ltd.), Liquistar EW-400 (trade name; Riken Vitamin Co., Ltd.) Products, such as pentaerythritol tetrastearate), Rikemar S-74 (trade name; manufactured by Riken Vitamin Co., Ltd., diglycerin tetrastearate), Rikemar TS-75 (trade name; Triglycerin pentastearate) manufactured by Riken Vitamin Co., etc. It can be mentioned.
  • a cosmetic composition containing the scrub agent of the present invention is also one form of the present invention.
  • the type of the cosmetic composition of the present invention is not particularly limited.
  • cleansing agents facial cleansers (face-washing foams, shaving foams, etc.), hand-washing agents (hand soaps, etc.), personal cleansing agents (body shampoos, shampoos, etc.) , Pack agents, body massage agents, body pack agents and the like.
  • the form of the cosmetic composition of the present invention is not particularly limited, and examples thereof include solid, liquid, emulsion, gel and cream.
  • the cosmetic composition of the present invention can be prepared by mixing the scrubbing agent of the present invention and other components usually used in cosmetics.
  • the amount of the scrubbing agent is preferably adjusted depending on the use, purpose, form and the like, but preferably 0.1 to 20% by mass, more preferably 1 to 10% in the cosmetic composition, for example. It is mass%. It is preferable that it is in the above-mentioned range because a moderate scrub feeling or a massage effect can be obtained.
  • the scrub agent in the case of a cleansing agent, can be blended in an amount of 0.1 to 20% by mass in the cosmetic composition, and further, a moisturizer, an oil, fatty acids, surfactants, alkaline substances, alcohols, Esters, anti-inflammatory agents, sequestering agents, vitamins, antioxidants, thickeners, purified water, pH adjusters, flavors, preservatives, bactericides, coloring agents, scrub agents other than the scrub agents of the present invention, etc. It can be selected appropriately and blended.
  • a moisturizer an oil, fatty acids, surfactants, alkaline substances, alcohols, Esters, anti-inflammatory agents, sequestering agents, vitamins, antioxidants, thickeners, purified water, pH adjusters, flavors, preservatives, bactericides, coloring agents, scrub agents other than the scrub agents of the present invention, etc. It can be selected appropriately and blended.
  • the cosmetic composition of the present invention contains the scrub agent of the present invention, it is possible to remove dirt on the skin effectively with low irritation without damaging the skin surface.
  • the cosmetic composition containing the scrub agent is washed away, it does not stay in the ecosystem for a long time in the natural world like synthetic resin particles (microbeads etc.) and accumulates further, so it has an adverse effect on the environment. The possibility of exerting is low.
  • Nitrogen was flowed at 0.5 ml / min and the temperature was raised to 230 ° C. while stirring.
  • the reaction was carried out at 230 ° C. for 5 hours, and after completion of the reaction, it was neutralized with 1.0 g (0.0086 mol) of phosphoric acid (trade name: phosphoric acid; manufactured by Wako Pure Chemical Industries, Ltd.) and the precipitate was removed by vacuum filtration.
  • the resulting reaction solution is heated and dissolved at 100 ° C. for 30 minutes, and then sprayed into an atomizing cooling tower cooled to -10 ° C. using an empty conical nozzle to coagulate to prepare powdered behenic acid triglyceride. did.
  • the resulting 12-hydroxystearic acid triglyceride was used as a scrub agent 19.
  • the median diameter and particle size distribution of the resulting scrub agents 1 to 19 were measured by a sonic vibration type fully automatic sieving particle size distribution measuring instrument (model: RPS-85; manufactured by Seishin Enterprise Co., Ltd.). Further, the hydroxyl value of the scrub agent (raw material) was measured according to the standard fat and oil analysis method 2.3.6.2-1996 hydroxyl value.
  • the cleansing foams 1 to 12 and 17 to 19 using the example products 1 to 15 as scrub agents had good cleansing effect and massage effect.
  • the cleansing foams 13 to 15 using the comparative products 1 to 3 as the scrub agents one or both of the cleansing effect and the massage effect were evaluated to be bad.
  • a scrub agent containing a polyhydric alcohol fatty acid ester having a relatively small hydroxyl value for example, 200 mg KOH / g or less, particularly 100 mg KOH / g or less, 80 mg KOH / g or less, etc.
  • a novel cosmetic scrub agent etc. can be provided.

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Abstract

Provided is a scrub agent for cosmetics, the scrub agent having, as a main component, a polyhydric alcohol fatty acid ester which is a chemically synthesizable synthetic wax. This scrub agent for cosmetics is characterized by being particles having a median diameter of 50-2000 μm and containing a polyhydric alcohol fatty acid ester having a melting point of at least 50 °C.

Description

化粧料用スクラブ剤Cosmetic scrub agent
 本発明は、クレンジング剤、洗顔料、手洗い剤、身体洗浄剤等の洗浄料、マッサージ料等の化粧料に用いるスクラブ剤に関する。 The present invention relates to a scrub agent used for a cleansing agent, a cleansing agent such as a cleansing agent, a face wash, a hand washing agent, a body cleansing agent, and a cosmetic agent such as a massage agent.
 従来より、洗浄料やマッサージ料等の化粧料には、皮膚の汚れや古い角質の除去、マッサージ効果を得ること等を目的としてスクラブ剤を配合している。従来のスクラブ剤としては、合成樹脂の粒子(マイクロビーズ等)、炭酸カルシウムの粒子、クルミやアンズ等の植物種子を粉砕した粒子、キャンデリラワックスやカルナウバロウ等の天然ワックスの粒子等が用いられている(特許文献1~5)。 Heretofore, scrubbing agents have been added to cosmetics such as cleansing agents and massage agents for the purpose of removing dirt from the skin and old keratin and obtaining a massage effect. As conventional scrubbing agents, particles of synthetic resin (microbeads etc.), particles of calcium carbonate, particles of crushed plant seeds such as walnut and apricot, particles of natural wax such as candelilla wax and carnauba wax, etc. are used. (Patent Documents 1 to 5).
 しかし、合成樹脂や炭酸カルシウム等は、自然界に排出されると長期にわたり残り続け、生態系にとどまり、更に蓄積することで様々な影響を及ぼす可能性がある。また、植物種子を粉砕した粒子は、不定形で鋭い割面を有するものが多いため、皮膚や目の角膜等を損傷するという問題を生ずる可能性がある。そして、天然ワックスの粒子は、天然ワックス自体が天然物であるために安定供給が難しく更に要求する性能に調整することが難しいという問題がある。そこで、自然環境や人体への悪影響が少なく、要求する性能に調整しやすい化学的に合成可能な合成ワックスであるスクラブ剤が求められていた。 However, synthetic resins and calcium carbonate, etc., if left in the natural world, will remain for a long time, stay in the ecosystem, and have various effects by further accumulating. In addition, many particles obtained by crushing plant seeds may cause problems such as damage to the skin or the cornea of the eye, because they have an irregular shape and a sharp fractured surface. The particles of natural wax have a problem that stable supply is difficult because the natural wax itself is a natural product, and it is difficult to adjust to the required performance. Therefore, there has been a demand for a scrubbing agent that is a chemically synthesizable synthetic wax that is less likely to adversely affect the natural environment or human body and can be easily adjusted to the required performance.
特開2000-247860号公報JP 2000-247860 A 特開2005-330472号公報JP 2005-330472 A 特開平10-338625号公報JP 10-338625 A 特開平9-249529号公報JP-A-9-249529 特開2004-189612号公報Japanese Patent Laid-Open No. 2004-189612
 本発明の目的は、化学的に合成可能な合成ワックスである多価アルコール脂肪酸エステルを主成分とする化粧料用スクラブ剤を提供することである。 An object of the present invention is to provide a cosmetic scrubbing agent comprising a polyhydric alcohol fatty acid ester, which is a chemically synthesized synthetic wax, as a main component.
 本発明者は、上記課題を解決するために鋭意研究を重ねた結果、化学的に合成した常温で固体の多価アルコール脂肪酸エステルを粒子とし、化粧料用スクラブ剤として用いることにより上記課題を解決することを見出した。本発明者は、これらの知見に基づき更に研究を重ね、本発明を完成するに至った。
 すなわち、本発明は、以下の構成を有する。
[1]メジアン径が50~2000μmであって、融点が50℃以上の多価アルコール脂肪酸エステルを含有する粒子であることを特徴とするスクラブ剤(例えば、化粧料用スクラブ剤)。
[2]多価アルコール脂肪酸エステルの水酸基価が200mgKOH/g以下(例えば、100mgKOH/g以下、特に80mgKOH/g以下)である上記[1]に記載のスクラブ剤。
[3]355μm以下(例えば、150~355μm程度)の粒子を、10%以上(例えば、30%以上、35%以上、40%以上)含む、上記[1]又は[2]に記載のスクラブ剤。
[4]洗顔料用である上記[1]~[3]のいずれかに記載のスクラブ剤。
[5]メジアン径が50~2000μm、融点が50℃以上の多価アルコール脂肪酸エステルを含有する粒子であり、355μm以下(例えば、150~355μm程度)の粒子を、10%以上(例えば、30%以上、35%以上、40%以上)含むことを特徴とするスクラブ剤(例えば、化粧料用スクラブ剤)。
[6]上記[1]~[5]のいずれかに記載のスクラブ剤(例えば、化粧料用スクラブ剤)を含有することを特徴とする化粧料組成物。
[7]上記[1]~[6]のいずれかに記載のスクラブ剤又は組成物を用いる、被対象部位(例えば、顔、体、手、全身等)の洗浄方法。
[8]上記[1]~[6]のいずれかに記載のスクラブ剤又は組成物を用いる、被対象部位(例えば、顔、体、手、全身等)のマッサージ方法。
[9]上記[1]~[6]のいずれかに記載のスクラブ剤又は組成物を用いる、被対象部位(例えば、顔、体、手、全身等)の洗浄及びマッサージ方法。
As a result of intensive studies to solve the above problems, the present inventor solves the above problems by using chemically synthesized normal temperature solid polyhydric alcohol fatty acid ester as particles and using it as a scrub agent for cosmetics. I found it to be. The present inventors have further studied based on these findings to complete the present invention.
That is, the present invention has the following configuration.
[1] A scrub agent (for example, a scrub agent for cosmetics), which is a particle containing a polyhydric alcohol fatty acid ester having a median diameter of 50 to 2000 μm and a melting point of 50 ° C. or higher.
[2] The scrub agent according to the above [1], wherein the hydroxyl value of the polyhydric alcohol fatty acid ester is 200 mg KOH / g or less (e.g., 100 mg KOH / g or less, particularly 80 mg KOH / g or less).
[3] The scrub agent according to the above [1] or [2], containing 10% or more (eg, 30% or more, 35% or more, 40% or more) of particles of 355 μm or less (eg, about 150 to 355 μm) .
[4] The scrub agent according to any one of the above [1] to [3], which is for use as a cleanser.
[5] A particle containing a polyhydric alcohol fatty acid ester having a median diameter of 50 to 2000 μm and a melting point of 50 ° C. or more, and particles of 355 μm or less (eg, about 150 to 355 μm) Above, 35% or more, 40% or more) containing scrub agent (for example, cosmetic scrub agent).
[6] A cosmetic composition comprising the scrub agent according to any one of the above [1] to [5] (for example, a cosmetic scrub agent).
[7] A method for cleaning a target site (eg, face, body, hands, whole body, etc.) using the scrub agent or composition according to any one of the above [1] to [6].
[8] A massage method for a target site (eg, face, body, hands, whole body, etc.) using the scrub agent or composition according to any one of the above [1] to [6].
[9] A method for cleaning and massaging a target site (eg, face, body, hands, whole body, etc.) using the scrub agent or composition according to any one of the above [1] to [6].
 本発明の化粧料用スクラブ剤は、化粧料組成物に用いることによって、従来用いられているスクラブ剤(合成樹脂の粒子)を用いた化粧料組成物と同程度の洗浄効果及びマッサージ効果を得ることができる。また、本発明の化粧料用スクラブ剤は、化学的に合成可能な合成ワックスである多価アルコール脂肪酸エステルを主成分とするので安定供給が可能であり、更に環境中に放出されても長期間にわたって残存することなく環境に対する悪影響が少ない。更に、本発明では、保存安定性に優れる化粧品用スクラブ剤を提供することもできる。 The scrub agent for cosmetics of the present invention achieves the same cleaning effect and massage effect as the cosmetic composition using the conventionally used scrub agent (particles of synthetic resin) by being used in the cosmetic composition. be able to. In addition, since the cosmetic scrub agent of the present invention is mainly composed of polyhydric alcohol fatty acid ester, which is a synthetic wax that can be synthesized chemically, stable supply is possible, and further it is possible to release it in the environment for a long time There is little adverse effect on the environment without remaining over Furthermore, the present invention can also provide a cosmetic scrubbing agent excellent in storage stability.
 本発明の化粧料用スクラブ剤(以下、単に「スクラブ剤」ともいう)は、主成分として融点が50℃以上の多価アルコール脂肪酸エステルを含有し、メジアン径が50~2000μmの粒子である。 The cosmetic scrub agent of the present invention (hereinafter, also simply referred to as "scrub agent") is a particle containing a polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more as a main component, and having a median diameter of 50 to 2000 μm.
 本発明で用いられる多価アルコール脂肪酸エステルは、多価アルコールと脂肪酸とがエステル結合した物質であり、化学的に合成可能な合成ワックスである。 The polyhydric alcohol fatty acid ester used in the present invention is a substance in which a polyhydric alcohol and a fatty acid are ester-bonded, and is a synthetic wax that can be chemically synthesized.
 上記多価アルコール脂肪酸エステルを構成する多価アルコールとしては、1分子中に水酸基が2個以上含むアルコールであれば特に制限はなく、例えば、エチレングリコール、1,3-プロパンジオール、プロピレングリコール、1,4-ブタンジオール、1,2-ブタンジオール、2-メチル-1,3-プロパンジオール、1,5-ペンタンジオール、ネオペンチルグリコール、1,6-ヘキサンジオール、2-エチル-2-メチル-1,3-プロパンジオール、1,7-ヘプタンジオール、2-メチル-2-プロピル-1,3-プロパンジオール、2,2-ジエチル-1,3-プロパンジオール、1,8-オクタンジオール、1,9-ノナンジオール、1,10-デカンジオール、1,11-ウンデカンジオール、1,12-ドデカンジオール等の二価アルコール;トリメチロールエタン、トリメチロールプロパン、トリメチロールブタン、ジトリメチロールプロパン、トリメチロールプロパン、ペンタエリスリトール、ジペンタエリスリトール、トリペンタエリスリトール、グリセリン、ポリグリセリン(グリセリンの2~20量体等)、1,3,5-ペンタントリオール、ソルビトール、ソルビタン、ソルビトールグリセリン縮合物、アドニトール、アラビトール、キシリトール、マンニトール等の三価以上の多価アルコール等が挙げられる。更に、キシロース、アラビノース、リボース、ラムノース、グルコース、フルクトース、ガラクトース、マンノース、ソルボース、セロビオース、マルトース、イソマルトース、トレハロース、シュクロース、ラフィノース、ゲンチアノース、メレンジトース等の三価以上の多価アルコールである糖類等も挙げられる。
 これらの多価アルコールのなかでも、グリセリン、ポリグリセリン;ソルビトール、ソルビタン;エチレングリコール、プロピレングリコール等のアルキレングリコール及びこれらの重合物;ペンタエリスリトール、ジペンタエリスリトール、トリメチロールプロパン等は入手が容易であり、多価アルコールと脂肪酸とをエステル化反応することが比較的容易であるため好ましい。これらの多価アルコールは、1種又は2種以上を併用してもよい。
The polyhydric alcohol constituting the polyhydric alcohol fatty acid ester is not particularly limited as long as it is an alcohol containing two or more hydroxyl groups in one molecule, and examples thereof include ethylene glycol, 1,3-propanediol, propylene glycol, 1 , 4-butanediol, 1,2-butanediol, 2-methyl-1,3-propanediol, 1,5-pentanediol, neopentyl glycol, 1,6-hexanediol, 2-ethyl-2-methyl- 1,3-propanediol, 1,7-heptanediol, 2-methyl-2-propyl-1,3-propanediol, 2,2-diethyl-1,3-propanediol, 1,8-octanediol, 1 , 9-nonanediol, 1,10-decanediol, 1,11-undecanediol, 1,12-dodecane Dihydric alcohols such as toluene; trimethylol ethane, trimethylol propane, trimethylol butane, di trimethylol propane, trimethylol propane, pentaerythritol, dipentaerythritol, tripentaerythritol, glycerin, polyglycerin (2 to 20 parts of glycerin) And the like), 1,3,5-pentanetriol, sorbitol, sorbitan, sorbitol-glycerin condensate, adonitol, arabitol, xylitol, trivalent or higher polyhydric alcohol such as mannitol, and the like. Furthermore, saccharides and the like which are trivalent or higher polyhydric alcohols such as xylose, arabinose, ribose, rhamnose, glucose, fructose, galactose, mannose, sorbose, cellobiose, maltose, isomaltose, trehalose, sucrose, raffinose, gentianose, melenditose, etc. Can also be mentioned.
Among these polyhydric alcohols, glycerin, polyglycerin; sorbitol, sorbitan; alkylene glycols such as ethylene glycol and propylene glycol and polymers thereof; pentaerythritol, dipentaerythritol, trimethylolpropane and the like are easily available. It is preferable because it is relatively easy to esterify the polyhydric alcohol and the fatty acid. These polyhydric alcohols may be used alone or in combination of two or more.
 上記多価アルコール脂肪酸エステルを構成する脂肪酸は、直鎖脂肪酸又は分岐脂肪酸であってもよく、更に飽和脂肪酸又は不飽和脂肪酸のいずれの脂肪酸であってもよいが、炭素数8~24の脂肪酸であることが好ましい。このような脂肪酸としては、例えば、カプリル酸、2-エチルヘキサン酸、イソノナン酸、カプリン酸、ラウリン酸、ミリスチン酸、イソミリスチン酸、パルミチン酸、イソパルミチン酸、ステアリン酸、イソステアリン酸、リシノレイン酸、オレイン酸、リノール酸、リノレン酸、アラキジン酸、イソアラキジン酸、ベヘン酸、エルカ酸等が挙げられる。これら脂肪酸の中でも、パルミチン酸、ステアリン酸、ベヘン酸等は、多価アルコール脂肪酸エステルとしたときに好適な融点を示しスクラブ効果が高いため好ましい。これら脂肪酸は1種又は2種以上を併用してもよい。 The fatty acid constituting the polyhydric alcohol fatty acid ester may be a linear fatty acid or a branched fatty acid, and may be any fatty acid of saturated fatty acid or unsaturated fatty acid, but is a fatty acid having 8 to 24 carbon atoms Is preferred. Such fatty acids include, for example, caprylic acid, 2-ethylhexanoic acid, isononanoic acid, capric acid, lauric acid, myristic acid, isomyristic acid, palmitic acid, isopalmic acid, stearic acid, isostearic acid, licinoleic acid, Oleic acid, linoleic acid, linolenic acid, arachidic acid, isoarachidic acid, behenic acid, erucic acid and the like can be mentioned. Among these fatty acids, palmitic acid, stearic acid, behenic acid and the like are preferable because when they are polyhydric alcohol fatty acid esters, they exhibit a suitable melting point and a high scrubbing effect. These fatty acids may be used alone or in combination of two or more.
 上記多価アルコール脂肪酸エステルの水酸基価は、特に限定されないが、好ましくは200mgKOH/g以下、より好ましくは100mgKOH/g以下、更により好ましくは80mgKOH/g以下であってもよく、50mgKOH/g以下(例えば、40mgKOH/g以下、30mgKOH/g以下、25mgKOH/g以下、20mgKOH/g以下等)であってもよい。このような水酸基価の多価アルコール脂肪酸エステルを使用することで、保存安定性に優れた化粧料組成物を効率よく得やすい。 The hydroxyl value of the polyhydric alcohol fatty acid ester is not particularly limited, but is preferably 200 mg KOH / g or less, more preferably 100 mg KOH / g or less, still more preferably 80 mg KOH / g or less, and 50 mg KOH / g or less For example, 40 mg KOH / g or less, 30 mg KOH / g or less, 25 mg KOH / g or less, 20 mg KOH / g or less, etc. may be used. By using such polyhydric alcohol fatty acid ester having a hydroxyl value, a cosmetic composition having excellent storage stability can be efficiently obtained.
 なお、多価アルコール脂肪酸エステルの水酸基価は、例えば、基準油脂分析法2.3.6.2‐1996 ヒドロキシル価に準じて測定できる。 In addition, the hydroxyl value of polyhydric-alcohol fatty acid ester can be measured according to the reference | standard fats-and-oils analysis 2.3.6.2-1996 hydroxyl value, for example.
 本発明で用いられる多価アルコール脂肪酸エステルは、融点が50℃以上であり、好ましくは60℃以上である。多価アルコール脂肪酸エステルの融点が50℃以上であると、使用時においてスクラブ剤として適度な硬さであるため好ましい。
 また、多価アルコール脂肪酸エステルの融点の上限としては特に制限はないが、好ましくは100℃以下、より好ましくは90℃以下、更により好ましくは80℃以下である。多価アルコール脂肪酸エステルの融点の上限が上記以下であると、粒子の形状に加工しやすいため好ましい。
The polyhydric alcohol fatty acid ester used in the present invention has a melting point of 50 ° C. or more, preferably 60 ° C. or more. It is preferable that the melting point of the polyhydric alcohol fatty acid ester is 50 ° C. or higher because the hardness is appropriate as a scrub agent at the time of use.
The upper limit of the melting point of the polyhydric alcohol fatty acid ester is not particularly limited, but is preferably 100 ° C. or less, more preferably 90 ° C. or less, and still more preferably 80 ° C. or less. When the upper limit of the melting point of the polyhydric alcohol fatty acid ester is below the above, it is preferable because it can be easily processed into the shape of particles.
 ここで、多価アルコール脂肪酸エステルの融点は、基準油脂分析法2.2.4.2-1996 融点(上昇融点)に基づいて測定することができる。 Here, the melting point of polyhydric alcohol fatty acid ester can be measured based on the standard fat and oil analysis method 2.2.4.2-1996 melting point (rising melting point).
 本発明で用いられる融点が50℃以上の多価アルコール脂肪酸エステルは、公知の方法で多価アルコールと脂肪酸とをエステル結合して製造することができ、例えば、反応器中に脂肪酸と多価アルコールを導入し、無触媒あるいは触媒存在下で、撹拌しながらエステル化反応させて多価アルコール脂肪酸エステルを製造することができる。前記反応の温度に特に制限はないが、例えば、150~300℃の温度範囲内で行なうのが好ましい。また、多価アルコール脂肪酸エステルの酸化劣化を防ぐため、反応器内を窒素パージしながらエステル化反応を行なうのが好ましい。エステル化反応後は、必要に応じて、未反応の脂肪酸や多価アルコールを除去するために、減圧留去や、アルカリ中和後の水洗処理等を行なっても良い。 The polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or higher used in the present invention can be produced by ester bonding a polyhydric alcohol and a fatty acid by a known method, for example, fatty acid and polyhydric alcohol in a reactor. Can be introduced into the reaction mixture and the esterification reaction can be carried out with stirring in the absence of a catalyst or in the presence of a catalyst to produce a polyhydric alcohol fatty acid ester. There is no particular limitation on the temperature of the reaction, but for example, it is preferable to carry out in the temperature range of 150 to 300 ° C. Further, in order to prevent oxidative degradation of polyhydric alcohol fatty acid ester, it is preferable to carry out the esterification reaction while purging the inside of the reactor with nitrogen. After the esterification reaction, if necessary, in order to remove unreacted fatty acid and polyhydric alcohol, distillation under reduced pressure or washing with water after neutralization with alkali may be performed.
 本発明のスクラブ剤は、スクラブ剤としての使用感、洗浄効果を発揮するために常温(0~30℃)で固体状の粒子である。そしてその粒子のメジアン径は50~2000μmであり、好ましくは100~1000μm、より好ましくは200~500μmである。 The scrub agent of the present invention is a solid particle at normal temperature (0 to 30 ° C.) in order to exert a feeling of use as a scrub agent and a cleaning effect. The median diameter of the particles is 50 to 2000 μm, preferably 100 to 1000 μm, and more preferably 200 to 500 μm.
 スクラブ剤の粒度分布は、特に限定されないが、所望の物性等に応じて、適宜選択してもよい。例えば、洗浄効果の観点から、355μm以下(例えば、150~355μm程度)の粒子を、好ましくは10%以上、より好ましくは30%以上(例えば、35%以上、40%以上)含むスクラブ剤としてもよい。
 また、355μm超(例えば、500μm以上、500μm超、850μm以上、850μm超等)の粒子を、好ましくは10%以上、より好ましくは30%以上(例えば、35%以上、40%以上)含むスクラブ剤としてもよい。
The particle size distribution of the scrubbing agent is not particularly limited, but may be appropriately selected depending on the desired physical properties and the like. For example, from the viewpoint of cleaning effect, it is also preferable as a scrub agent containing particles of 355 μm or less (eg, about 150 to 355 μm), preferably 10% or more, more preferably 30% or more (eg 35% or more, 40% or more). Good.
Also, a scrub agent containing particles of 355 μm or more (eg, 500 μm or more, 500 μm or more, 850 μm or more, 850 μm or more), preferably 10% or more, more preferably 30% or more (eg 35% or more, 40% or more) It may be
 ここでメジアン径とは、体積基準での積算分布曲線の50%に相当する平均粒子径(d50)である。メジアン径や粒度分布は、例えば、音波振動式全自動ふるい分け粒度分布測定器(型式:RPS-85;セイシン企業製)等で測定することができる。 Here, the median diameter is an average particle diameter (d50) corresponding to 50% of the integrated distribution curve on a volume basis. The median diameter and the particle size distribution can be measured, for example, by a sonic vibration type fully automatic sieving particle size distribution measuring instrument (model: RPS-85; manufactured by Seishin Co., Ltd.).
 本発明のスクラブ剤は、上述の様に主成分として融点が50℃以上の多価アルコール脂肪酸エステルを含有している。ここで「主成分」とは、例えば、スクラブ剤中に融点が50℃以上の多価アルコール脂肪酸エステルが70質量%以上を占めることを意味し、好ましくは80質量%以上、より好ましくは90質量%以上、更により好ましくは95質量%以上である。 The scrub agent of the present invention contains polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more as a main component as described above. Here, “main component” means, for example, that 70% by mass or more of polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more is contained in the scrub agent, preferably 80% by mass or more, and more preferably 90% by mass. % Or more, still more preferably 95% by mass or more.
 本発明のスクラブ剤には、主成分である融点が50℃以上の多価アルコール脂肪酸エステルの他に、本発明の効果を阻害しない範囲でその他の成分を含有してもよく、例えば、炭化水素ワックス、天然ワックス等が挙げられる。上記炭化水素ワックスとしては、ポリエチレンワックス、ポリプロピレンワックス、マイクロクリスタリンワックス、パラフィンワックス、フィッシャートロプシュワックス等やこれらのカルボン酸変性ワックスが挙げられ、天然ワックスとしては、カルナウバワックス、キャンデリラワックス、ライスワックス、みつろう、モンタンワックス等が挙げられる。 The scrub agent of the present invention may contain, in addition to the polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more as the main component, other components in the range not to inhibit the effects of the present invention. Wax, natural wax and the like can be mentioned. Examples of the hydrocarbon wax include polyethylene wax, polypropylene wax, microcrystalline wax, paraffin wax, Fischer-Tropsch wax and the like, and carboxylic acid-modified waxes thereof, and natural waxes such as carnauba wax, candelilla wax, rice wax And beeswax, montan wax and the like.
 本発明のスクラブ剤の製造方法に特に制限はないが、例えば、融点が50℃以上の多価アルコール脂肪酸エステルと所望によりその他の成分とを加熱等して溶液状の混合物を作製した後、冷却して固体状としてから粉砕機等で粉砕、整粒等して粒子状のスクラブ剤を製造する方法、上記溶液状の混合物をそのまま冷気中にスプレー等して凝固させて粒子状のスクラブ剤を製造する方法、上記溶液状の混合物と水、賦形剤(デキストリン、カゼインナトリウム等)等を加え乳化した後、スプレードライして粒子状のスクラブ剤を製造する方法等、公知の方法を採用することができる。
 更に、得られた粒子状のスクラブ剤を造粒、ふるい分け等することにより目的に応じた粒子径を有するスクラブ剤を製造することもできる。上記造粒方法に特に制限はないが、例えば、撹拌造粒法、流動層造粒法、押出造粒法、転動造粒法、圧縮造粒法等の公知の方法を採用することができる。
The method for producing the scrub agent of the present invention is not particularly limited. For example, a polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or higher and optionally other components are heated to prepare a solution mixture, and then cooled. And solidify and then pulverize and size the particles with a grinder or the like to produce a particulate scrub agent, the above mixture in solution form is directly sprayed in cold air to coagulate the particulate scrub agent. A known method such as a method of producing, a method of producing a particulate scrub agent after spray-drying after adding the above solution mixture and water, an excipient (dextrin, casein sodium etc.), etc. and emulsifying is used. be able to.
Furthermore, it is also possible to produce a scrub agent having a particle diameter according to the purpose by granulating, sieving, etc. the obtained particulate scrub agent. The above granulation method is not particularly limited, but, for example, known methods such as stirring granulation method, fluidized bed granulation method, extrusion granulation method, rolling granulation method, compression granulation method and the like can be adopted. .
 本発明のスクラブ剤の形状としては、メジアン径が50~2000μmの粒子であれば特に制限はないが、例えば、球状、楕円状、鱗片状、フレーク状、板状、棒状、針状等のいずれの形状であってもよい。また、本発明のスクラブ剤の構造に特に制限はないが、例えば、崩壊性等を考慮したスクラブ剤中に空間を有するポーラスな構造、又は空間を有さない密な構造等であってもよい。 The shape of the scrub agent of the present invention is not particularly limited as long as it is a particle having a median diameter of 50 to 2000 μm, for example, any of spherical, elliptical, scaly, flake, plate, rod, needle, etc. It may be in the form of Further, the structure of the scrub agent of the present invention is not particularly limited, but may be, for example, a porous structure having a space in the scrub agent considering disintegrability etc., or a dense structure having no space, etc. .
 本発明のスクラブ剤は、市販の融点が50℃以上の多価アルコール脂肪酸エステルをそのまま、或いはふるい分け等して目的に応じた粒子径にして用いることが可能である。市販の融点が50℃以上の多価アルコール脂肪酸エステルとしては、例えば、リケマールTG-12(商品名;理研ビタミン社製、12-ヒドロキシステアリン酸トリグリセリド)、リケスターEW-400(商品名;理研ビタミン社製、テトラステアリン酸ペンタエリスリトール)、リケマールS-74(商品名;理研ビタミン社製、テトラステアリン酸ジグリセリン)、リケマールTS-75(商品名;理研ビタミン社製、ペンタステアリン酸トリグリセリン)等が挙げられる。 The scrubbing agent of the present invention can be used as a commercially available polyhydric alcohol fatty acid ester having a melting point of 50 ° C. or more, as it is or by sieving, etc., to a particle diameter according to the purpose. Commercially available polyhydric alcohol fatty acid esters having a melting point of 50 ° C. or higher include, for example, Rikemar TG-12 (trade name; 12-hydroxystearic acid triglyceride manufactured by Riken Vitamin Co., Ltd.), Liquistar EW-400 (trade name; Riken Vitamin Co., Ltd.) Products, such as pentaerythritol tetrastearate), Rikemar S-74 (trade name; manufactured by Riken Vitamin Co., Ltd., diglycerin tetrastearate), Rikemar TS-75 (trade name; Triglycerin pentastearate) manufactured by Riken Vitamin Co., etc. It can be mentioned.
 本発明のスクラブ剤を含有する化粧料組成物も本発明の形態の1つである。
 本発明の化粧料組成物の種類に特に制限はないが、例えば、クレンジング剤、洗顔料(洗顔フォーム、シェービングフォーム等)、手洗い剤(ハンドソープ等)、身体洗浄剤(ボディシャンプー、シャンプー等)、パック剤、ボディーマッサージ剤、ボディ用パック剤等が挙げられる。
 本発明の化粧料組成物の剤型に特に限定はないが、例えば、固形物、液状、乳液状、ジェル状、クリーム状等の剤型が挙げられる。
A cosmetic composition containing the scrub agent of the present invention is also one form of the present invention.
The type of the cosmetic composition of the present invention is not particularly limited. For example, cleansing agents, facial cleansers (face-washing foams, shaving foams, etc.), hand-washing agents (hand soaps, etc.), personal cleansing agents (body shampoos, shampoos, etc.) , Pack agents, body massage agents, body pack agents and the like.
The form of the cosmetic composition of the present invention is not particularly limited, and examples thereof include solid, liquid, emulsion, gel and cream.
 本発明の化粧料組成物は、本発明のスクラブ剤とその他の通常化粧料に用いられる成分とを混合して調製することができる。スクラブ剤の配合量は、それぞれの用途、目的及び形態等によって異なるので適宜調整することが望ましいが、例えば、化粧料組成物中に好ましくは0.1~20質量%、より好ましくは1~10質量%である。上記範囲内であると、適度なスクラブ感、或いはマッサージ効果が得られるので好ましい。 The cosmetic composition of the present invention can be prepared by mixing the scrubbing agent of the present invention and other components usually used in cosmetics. The amount of the scrubbing agent is preferably adjusted depending on the use, purpose, form and the like, but preferably 0.1 to 20% by mass, more preferably 1 to 10% in the cosmetic composition, for example. It is mass%. It is preferable that it is in the above-mentioned range because a moderate scrub feeling or a massage effect can be obtained.
 例えば、クレンジング料であれば、スクラブ剤は化粧料組成物中に0.1~20質量%を配合することができ、更に保湿剤、油剤、脂肪酸類、界面活性剤、アルカリ物質、アルコール類、エステル類、消炎剤、金属封鎖剤、ビタミン類、酸化防止剤、増粘剤、精製水、pH調節剤、香料、防腐剤、殺菌剤、着色料、本発明のスクラブ剤以外のスクラブ剤等を適宜選択して配合することができる。 For example, in the case of a cleansing agent, the scrub agent can be blended in an amount of 0.1 to 20% by mass in the cosmetic composition, and further, a moisturizer, an oil, fatty acids, surfactants, alkaline substances, alcohols, Esters, anti-inflammatory agents, sequestering agents, vitamins, antioxidants, thickeners, purified water, pH adjusters, flavors, preservatives, bactericides, coloring agents, scrub agents other than the scrub agents of the present invention, etc. It can be selected appropriately and blended.
 本発明の化粧料組成物は、本発明のスクラブ剤を含有しているので、皮膚表面を傷つけることなく低刺激で効果的に皮膚上の汚れを取り除くことができる。また、スクラブ剤を含有する化粧料組成物を洗い流しても、合成樹脂の粒子(マイクロビーズ等)の様に自然界に長期にわたり生態系にとどまり、更に蓄積することはないので、環境に対して悪影響を及ぼす可能性が低い。 Since the cosmetic composition of the present invention contains the scrub agent of the present invention, it is possible to remove dirt on the skin effectively with low irritation without damaging the skin surface. In addition, even if the cosmetic composition containing the scrub agent is washed away, it does not stay in the ecosystem for a long time in the natural world like synthetic resin particles (microbeads etc.) and accumulates further, so it has an adverse effect on the environment. The possibility of exerting is low.
 以下に本発明を実施例で説明するが、これは本発明を単に説明するだけのものであって、本発明を限定するものではない。 The invention will now be described by way of example, which is merely illustrative of the invention and is not limiting.
<スクラブ剤の作製>
(1)原材料
[多価アルコール脂肪酸エステル(粉末状)]
12-ヒドロキシステアリン酸トリグリセリド(商品名:リケマールTG-12;理研ビタミン社製)
テトラステアリン酸ペンタエリスリトール(商品名:リケスターEW-400;理研ビタミン社製)
テトラステアリン酸ジグリセリン(商品名:リケマールS-74;理研ビタミン社製)
ペンタステアリン酸トリグリセリン(商品名:リケマールTS-75;理研ビタミン社製)
ステアリン酸モノグリセリド(商品名:リケマールS-100P;理研ビタミン社製)
ステアリン酸プロピレングリコール(商品名;リケマールPS-100;理研ビタミン社製)
多価アルコール脂肪酸エステル混合物(下記の作製方法で作製したもの)
パームステアリン酸トリグリセリド(商品名:スプレーファットPM;理研ビタミン社製)
[合成樹脂(マイクロビーズ)]
ポリエチレン(商品名:フロービーズ;住友精化社製)
 上記各原材料の融点については、基準油脂分析法2.2.4.2-1996 融点(上昇融点)に基づいて測定した。結果を表1に示す。
<Preparation of scrub agent>
(1) Raw materials [polyhydric alcohol fatty acid ester (powdery)]
12-hydroxystearic acid triglyceride (trade name: Rikemar TG-12; manufactured by Riken Vitamin Co., Ltd.)
Pentaerythritol tetrastearate (trade name: Liquestar EW-400; manufactured by Riken Vitamin Co., Ltd.)
Tetrastearic acid diglycerin (trade name: Rikemar S-74; manufactured by Riken Vitamin Co., Ltd.)
Triglycerin pentastearate (trade name: Rikemar TS-75; manufactured by Riken Vitamin Co., Ltd.)
Stearic acid monoglyceride (trade name: Rikemar S-100P; manufactured by Riken Vitamin Co., Ltd.)
Propylene glycol stearate (trade name; Rikemar PS-100; manufactured by Riken Vitamin Co., Ltd.)
Polyhydric alcohol fatty acid ester mixture (made by the following method)
Palm stearic acid triglyceride (trade name: Spray Fat PM; manufactured by Riken Vitamin Co., Ltd.)
[Synthetic resin (micro beads)]
Polyethylene (trade name: Flow beads; manufactured by Sumitomo Seika Chemicals Co., Ltd.)
The melting points of the above-mentioned respective raw materials were measured based on the standard fat and oil analysis method 2.2.4.2-1996 melting point (rising melting point). The results are shown in Table 1.
(2-1)多価アルコール脂肪酸エステル混合物1(12-ヒドロキシステアリン酸トリグリセリドとステアリン酸プロピレングリコールの混合物)の作製方法
 12-ヒドロキシステアリン酸トリグリセリド(商品名:リケマールTG-12;理研ビタミン社製)8kgとステアリン酸プロピレングリコール(商品名;リケマールPS-100;理研ビタミン社製)2kgを混合し、100℃にて30分間加温溶解した後、-10℃に冷却した噴霧冷却塔中に噴霧して凝固し、粉末状の多価アルコール脂肪酸エステル混合物1を作製した。
(2-1) Method of preparing polyhydric alcohol fatty acid ester mixture 1 (mixture of 12-hydroxystearic acid triglyceride and propylene glycol stearate) 12-hydroxystearic acid triglyceride (trade name: Rikemar TG-12; manufactured by Riken Vitamin Co., Ltd.) 8 kg and 2 kg of propylene glycol stearate (trade name: Rikemar PS-100; manufactured by Riken Vitamins Co., Ltd.) are mixed and dissolved by heating at 100 ° C. for 30 minutes, and then sprayed into a spray cooling tower cooled to -10 ° C. The mixture was solidified to prepare powdery polyhydric alcohol fatty acid ester mixture 1.
(2-2)ベへニン酸トリグリセリドの作製方法
 温度計、窒素導入管、留分受器、攪拌棒を備えた2000mlの4ツ口フラスコ中にベヘニン酸(商品名:NAA‐222S;日油社製)1020g(3.0モル)、グリセリン(商品名:精製グリセリン;阪本薬品社製)92g(1.0モル)を仕込み触媒として酸化スズ(商品名:酸化すず(II);和光純薬社製)1.0g(0.0075モル)を加えた。窒素を0.5ml/minで流し、攪拌しながら230℃まで昇温した。230℃で5時間反応し、反応終了後、燐酸(商品名:りん酸;和光純薬社製)1.0g(0.0086モル)で中和し沈殿物を減圧濾過により除去した。得られた反応液を100℃にて30分間加温溶解した後、-10℃に冷却した噴霧冷却塔中に空円錐ノズルを用いて噴霧し、凝固させ粉末状のベへニン酸トリグリセリドを作製した。
(2-2) Preparation method of behenic acid triglyceride Behenic acid (trade name: NAA-222S; NOF Corporation in a 2000 ml four-necked flask equipped with a thermometer, a nitrogen introducing pipe, a fraction receiver, and a stirring rod) Co., Ltd .: 1020 g (3.0 mol), glycerin (trade name: refined glycerin; manufactured by Sakamoto Yakuhin Co., Ltd.) 92 g (1.0 mol) as a catalyst, tin oxide (trade name: tin oxide (II); Wako Pure Chemical Industries, Ltd. Co., Ltd. 1.0g (0.0075 mol) was added. Nitrogen was flowed at 0.5 ml / min and the temperature was raised to 230 ° C. while stirring. The reaction was carried out at 230 ° C. for 5 hours, and after completion of the reaction, it was neutralized with 1.0 g (0.0086 mol) of phosphoric acid (trade name: phosphoric acid; manufactured by Wako Pure Chemical Industries, Ltd.) and the precipitate was removed by vacuum filtration. The resulting reaction solution is heated and dissolved at 100 ° C. for 30 minutes, and then sprayed into an atomizing cooling tower cooled to -10 ° C. using an empty conical nozzle to coagulate to prepare powdered behenic acid triglyceride. did.
(2-3)多価アルコール脂肪酸エステル混合物2(12-ヒドロキシステアリン酸トリグリセリドとベへニン酸トリグリセリドの混合物)の作製方法
 上記方法で得られたべへニン酸トリグリセリド550gと12-ヒドロキシステアリン酸トリグリセリド450gを混合し、100℃にて30分間加温溶解した後、-10℃に冷却した噴霧冷却塔中に空円錐ノズルを用いて噴霧し、凝固させて粉末状の多価アルコール脂肪酸エステル混合物2を作製した。
(2-3) Method of preparing polyhydric alcohol fatty acid ester mixture 2 (mixture of 12-hydroxystearic acid triglyceride and behenic acid triglyceride) 550 g of behenic acid triglyceride obtained by the above method and 450 g of 12-hydroxystearic acid triglyceride The mixture is heated and dissolved at 100 ° C. for 30 minutes, and then sprayed into an atomizing cooling tower cooled to −10 ° C. using an empty conical nozzle to coagulate to form powdered polyhydric alcohol fatty acid ester mixture 2 Made.
(3)スクラブ剤の作製方法
 上記原材料のそれぞれをサニタリー振動ふるい(形式:SF-300;三庄インダストリー社製)を用いてふるい分けし、ふるい分けしたものを目的の粒径になるように適宜組合せて粒径を調整してスクラブ剤1~16を作製した。
 また、スクラブ剤17~18には、上記(2-2)又は(2-3)で得られた粉末をそのまま用いた。
 更に、12-ヒドロキシステアリン酸トリグリセリド1000gを混合し、100℃にて30分間加温溶解した後、-10℃に冷却した噴霧冷却塔中に空円錐ノズルを用いて噴霧し、凝固させて粉末状の12-ヒドロキシステアリン酸トリグリセリドを作製したものを、スクラブ剤19として用いた。
 得られたスクラブ剤1~19のメジアン径及び粒径分布については、音波振動式全自動ふるい分け粒度分布測定器(型式:RPS-85;セイシン企業社製)で測定した。
 また、スクラブ剤(原材料)の水酸基価を、基準油脂分析法2.3.6.2-1996 ヒドロキシル価に準じて測定した。
(3) Scrub agent preparation method Each of the above raw materials is sifted using a sanitary vibrating sieve (type: SF-300; manufactured by Mitaka Ind. Co., Ltd.), and those sifted are appropriately combined so as to obtain the desired particle size. The particle size was adjusted to prepare scrub agents 1-16.
Further, the powders obtained in the above (2-2) or (2-3) were used as the scrub agents 17 to 18 as they were.
Furthermore, 1000 g of 12-hydroxystearic acid triglyceride is mixed, heated and dissolved at 100 ° C. for 30 minutes, and then sprayed into an atomizing cooling tower cooled to -10 ° C. using an empty conical nozzle to coagulate and form powder The resulting 12-hydroxystearic acid triglyceride was used as a scrub agent 19.
The median diameter and particle size distribution of the resulting scrub agents 1 to 19 were measured by a sonic vibration type fully automatic sieving particle size distribution measuring instrument (model: RPS-85; manufactured by Seishin Enterprise Co., Ltd.).
Further, the hydroxyl value of the scrub agent (raw material) was measured according to the standard fat and oil analysis method 2.3.6.2-1996 hydroxyl value.
 結果を表1に示す。また、スクラブ剤の粒径分布を表2に示す。なお、表中、粒径範囲の「-A」とはAμm以下、「B-C」とは「Bμm超Cμm以下」、「D-」とは「Dμm超」を意味する。 The results are shown in Table 1. Also, the particle size distribution of the scrub agent is shown in Table 2. In the table, "-A" in the particle diameter range means A μm or less, "BC" means "more than B μm and C μm or less", and "D-" means "more than D μm".
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
<化粧料用組成物(洗顔フォーム)Aの作製>
 上記方法で得られたスクラブ剤1~16を用い下記の表3に示した配合で洗顔フォームAを下記方法でそれぞれ200g作製した。
 原材料Aを全て加えて80℃で加温溶解し、別途原材料Bを室温で溶解した。原材料Aの混合物を80℃に保ち、更に撹拌しながら原材料Bの混合物を徐々に加え、均一に溶解した。撹拌しながら冷却し、60℃になった時点で原材料Cを加え引き続き撹拌しながら35℃まで冷却し、攪拌をやめて室温(約25℃)になるまで放冷し化粧料組成物(洗顔フォーム1~16)を得た。
<Preparation of cosmetic composition (face-washing foam) A>
Using the scrub agents 1 to 16 obtained by the above method, 200 g of facial cleansing foam A was produced by the following method according to the formulation shown in Table 3 below.
The raw material A was all added and dissolved by heating at 80 ° C., and the raw material B was separately dissolved at room temperature. The mixture of raw materials A was kept at 80 ° C., and the mixture of raw materials B was gradually added with further stirring, and was uniformly dissolved. Cool with stirring, and at 60 ° C, add raw material C and continue cooling with stirring to 35 ° C, stop stirring and allow to cool to room temperature (about 25 ° C) and cosmetic composition (face wash foam 1 I got ~ 16).
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
<化粧料用組成物(洗顔フォーム)Bの作製>
 上記方法で得られたスクラブ剤17~19を用いて、下記の表4に示した配合で洗顔フォーム(アミノ酸系洗顔フォーム)Bを下記方法でそれぞれ200g作製した。
 全原材料を80℃で加温溶解し、撹拌しながら冷却して35℃まで冷却し、撹拌をやめて室温(約25℃)になるまで放冷し化粧料組成物(アミノ酸系洗顔フォーム:洗顔フォーム17~19)を得た。
<Preparation of cosmetic composition (face-washing foam) B>
Using the scrub agents 17 to 19 obtained by the above-mentioned method, 200 g of face-washing foam (amino acid-based face-washing foam) B was produced by the following method according to the composition shown in Table 4 below.
The whole raw material is dissolved by heating at 80 ° C, cooled with stirring and cooled to 35 ° C, and the stirring is stopped and allowed to cool to room temperature (about 25 ° C) and cosmetic composition (amino acid-based facial cleansing foam: facial cleansing foam 17 to 19) were obtained.
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
<スクラブ剤を用いた洗顔フォームの評価>
[評価方法]
 上記で得られた洗顔フォーム1~19(実施例品1~15、比較例品1~3、参考例品1のいずれかを配合)5gを手に取り、顔面に塗布して手指で30秒間マッサージし、洗浄効果、マッサージ効果及び保存安定性を表5の評価基準で評価した。尚、評価は男女パネラー20名にて行った。各パネラーが評価した評価点の平均点値を下記基準で記号化した。結果を表6に示す。
[記号化]
◎:評価点の平均値が3.5以上。
○:評価点の平均値が2.5以上、3.5未満。
△:評価点の平均値が1.5以上、2.5未満。
×:評価点の平均値が1.5未満。
<Evaluation of face wash foam using scrub agent>
[Evaluation method]
Take 5 g of the face-washing foam 1 to 19 (containing any of Examples 1 to 15, Comparative Examples 1 to 3, and Reference Example 1) obtained above, apply it to the face, and apply for 30 seconds with your fingers. It massaged and the cleaning effect, the massage effect, and storage stability were evaluated by the evaluation criteria of Table 5. The evaluation was conducted by 20 male and female panelists. The average point value of the evaluation point evaluated by each panelist was symbolized according to the following criteria. The results are shown in Table 6.
[Symbolization]
◎: The average value of evaluation points is 3.5 or more.
○: The average value of the rating points is 2.5 or more and less than 3.5.
Fair: Average value of evaluation points is 1.5 or more and less than 2.5.
X: The average value of evaluation points is less than 1.5.
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000006
 結果より、スクラブ剤として実施例品1~15を用いた洗顔フォーム1~12及び17~19は、洗顔効果及びマッサージ効果が良好であった。一方、スクラブ剤として比較例品1~3を用いた洗顔フォーム13~15は、洗顔効果及びマッサージ効果のいずれか、或いは両方が悪い評価であった。また、比較的水酸基価の小さい(例えば、200mgKOH/g以下、特に100mgKOH/g以下、80mgKOH/g以下等)多価アルコール脂肪酸エステル含有するスクラブ剤を用いることで、保存安定性に優れる洗顔フォームを効率よく得ることができた。
Figure JPOXMLDOC01-appb-T000006
From the results, it was found that the cleansing foams 1 to 12 and 17 to 19 using the example products 1 to 15 as scrub agents had good cleansing effect and massage effect. On the other hand, in the case of the cleansing foams 13 to 15 using the comparative products 1 to 3 as the scrub agents, one or both of the cleansing effect and the massage effect were evaluated to be bad. In addition, by using a scrub agent containing a polyhydric alcohol fatty acid ester having a relatively small hydroxyl value (for example, 200 mg KOH / g or less, particularly 100 mg KOH / g or less, 80 mg KOH / g or less, etc.) I was able to get it efficiently.
 本発明によれば、新規な化粧料用のスクラブ剤等を提供できる。 According to the present invention, a novel cosmetic scrub agent etc. can be provided.

Claims (2)

  1.  メジアン径が50~2000μmであって、融点が50℃以上の多価アルコール脂肪酸エステルを含有する粒子であることを特徴とする化粧料用スクラブ剤。 A scrub agent for cosmetics characterized in being particles containing a polyhydric alcohol fatty acid ester having a median diameter of 50 to 2000 μm and a melting point of 50 ° C. or higher.
  2.  請求項1に記載の化粧料用スクラブ剤を含有することを特徴とする化粧料組成物。 A cosmetic composition comprising the cosmetic scrub agent according to claim 1.
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