JP7555913B2 - Composite surface-treated inorganic powder and its manufacturing method, oil dispersion and cosmetic containing the inorganic powder - Google Patents
Composite surface-treated inorganic powder and its manufacturing method, oil dispersion and cosmetic containing the inorganic powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims description 136
- 239000002131 composite material Substances 0.000 title claims description 55
- 239000002537 cosmetic Substances 0.000 title claims description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000004533 oil dispersion Substances 0.000 title description 6
- 239000002245 particle Substances 0.000 claims description 49
- 238000004381 surface treatment Methods 0.000 claims description 34
- 239000003093 cationic surfactant Substances 0.000 claims description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 229920001296 polysiloxane Polymers 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 19
- REZZEXDLIUJMMS-UHFFFAOYSA-M dimethyldioctadecylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC REZZEXDLIUJMMS-UHFFFAOYSA-M 0.000 claims description 15
- 229910010272 inorganic material Inorganic materials 0.000 claims description 14
- 239000011147 inorganic material Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- 239000004664 distearyldimethylammonium chloride (DHTDMAC) Substances 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 5
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 4
- YSJGOMATDFSEED-UHFFFAOYSA-M behentrimonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCCCCCC[N+](C)(C)C YSJGOMATDFSEED-UHFFFAOYSA-M 0.000 claims description 4
- 229960000686 benzalkonium chloride Drugs 0.000 claims description 4
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 4
- IQDGSYLLQPDQDV-UHFFFAOYSA-N dimethylazanium;chloride Chemical compound Cl.CNC IQDGSYLLQPDQDV-UHFFFAOYSA-N 0.000 claims description 4
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- QMGAJHYFGBHHRR-UHFFFAOYSA-M trimethyl(3-octadecoxypropyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCCOCCC[N+](C)(C)C QMGAJHYFGBHHRR-UHFFFAOYSA-M 0.000 claims description 4
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 claims 2
- 230000000052 comparative effect Effects 0.000 description 24
- 239000012508 resin bead Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 14
- 239000012756 surface treatment agent Substances 0.000 description 12
- 238000011156 evaluation Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 238000006073 displacement reaction Methods 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 229920002050 silicone resin Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229920000426 Microplastic Polymers 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 2
- XIWFQDBQMCDYJT-UHFFFAOYSA-M benzyl-dimethyl-tridecylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 XIWFQDBQMCDYJT-UHFFFAOYSA-M 0.000 description 2
- 229940008099 dimethicone Drugs 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- 239000013500 performance material Substances 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000000475 sunscreen effect Effects 0.000 description 2
- 239000000516 sunscreening agent Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000013523 DOWSIL™ Substances 0.000 description 1
- 229920013731 Dowsil Polymers 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229920004482 WACKER® Polymers 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008271 cosmetic emulsion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 210000000245 forearm Anatomy 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 230000003655 tactile properties Effects 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/41—Amines
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/89—Polysiloxanes
- A61K8/896—Polysiloxanes containing atoms other than silicon, carbon, oxygen and hydrogen, e.g. dimethicone copolyol phosphate
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/12—Face or body powders for grooming, adorning or absorbing
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Chemical & Material Sciences (AREA)
- Dermatology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Cosmetics (AREA)
Description
本発明は、無機材料を主体とする基材粉体を特定の化合物で表面処理して得られる複合表面処理無機粉体に関し、特に基材粉体をカチオン界面活性剤及びアミノ変性シリコーンで表面処理することにより、樹脂ビーズと同等の柔らかさを備え、肌への付着性に優れた複合表面処理無機粉体及びその製造方法、その無機粉体が配合されている油性分散体及び化粧料に関する。 The present invention relates to a composite surface-treated inorganic powder obtained by surface-treating a base powder mainly made of an inorganic material with a specific compound, and in particular to a composite surface-treated inorganic powder obtained by surface-treating the base powder with a cationic surfactant and an amino-modified silicone, which has softness equivalent to that of resin beads and excellent adhesion to the skin, a method for producing the same, and an oil-based dispersion and cosmetic composition containing the inorganic powder.
従来より、多くの化粧料には、柔らかさ、しっとり感やさらさら感といった感触を与えることにより、使用時の感触を向上させる目的で、ナイロンパウダーやシリコーンビーズなどの樹脂ビーズ(マイクロプラスチックの一種)が配合されている。しかしながら、近年、マイクロプラスチックによる海洋環境の汚染が問題視されるようになっていることから、マイクロプラスチックを含有しない化粧料が求められている。 Traditionally, many cosmetics have been formulated with nylon powder or resin beads such as silicone beads (a type of microplastic) to improve the feel during use by imparting softness, moisture, and a smooth texture. However, in recent years, pollution of the marine environment by microplastics has become a problem, and there is a demand for cosmetics that do not contain microplastics.
このため、使用感を向上させる目的で化粧料に配合する樹脂ビーズ以外の粉体材料としては、例えば特開2004-182729号公報(特許文献1)、特開2009-062324号公報(特許文献2)に記載されているように、アミノ変性シリコーンで表面処理した粉体が開発されている。また同様に、例えば特開2008-291026号公報(特許文献3)に記載されているように、カチオン界面活性剤を吸着させた粉体も開発されている。For this reason, as powder materials other than resin beads that are blended into cosmetics to improve the feel when used, for example, powders that are surface-treated with amino-modified silicone have been developed, as described in JP-A No. 2004-182729 (Patent Document 1) and JP-A No. 2009-062324 (Patent Document 2). Similarly, powders that have adsorbed cationic surfactants have also been developed, as described in JP-A No. 2008-291026 (Patent Document 3).
しかしながら、特許文献1~3に記載された化粧料配合用の粉体は、上述した樹脂ビーズに比べると、柔らかさ、しっとり感やさらさら感といった使用感において十分に満足のいくものではなく、特に樹脂ビーズ特有の柔らかさを得られないという問題があった。However, the powders for incorporation into cosmetics described in Patent Documents 1 to 3 are not fully satisfactory in terms of feel when used, such as softness, moist feeling, and smooth feeling, compared to the resin beads mentioned above, and there is a particular problem in that they do not provide the softness characteristic of resin beads.
そこで、本発明は、上記事情を鑑みてなされたものであり、樹脂ビーズと同等又はそれ以上の感触を化粧料に付与することが可能な化粧料用粉体及びその製造方法を提供すること、若しくは当該材料を油性分散体又は化粧料に配合することにより、樹脂ビーズを配合することなく使用時の感触に優れる油性分散体又は化粧料を提供することを目的とする。Therefore, the present invention has been made in consideration of the above circumstances, and aims to provide a powder for cosmetics that can impart a feel to cosmetics that is equal to or better than that of resin beads, and a method for producing the same, or to provide an oil dispersion or cosmetic that has an excellent feel when used without incorporating resin beads, by incorporating the material into an oil dispersion or cosmetic.
本発明者等は、樹脂ビーズと同等又はそれ以上の感触を化粧料に付与することができる代替材料及びその表面処理材料などについて鋭意研究を重ねた結果、無機材料を主体とする基材粉体にカチオン界面活性剤及びアミノ変性シリコーンを表面処理すれば、樹脂ビーズと同等又はそれ以上の性能を有する複合表面処理無機粉体を得られることを見出し、本発明を完成するに至った。As a result of extensive research into alternative materials and surface treatment materials for them that can impart a feel to cosmetics equal to or greater than that of resin beads, the inventors discovered that by surface-treating a base powder mainly made of inorganic material with a cationic surfactant and amino-modified silicone, a composite surface-treated inorganic powder with performance equal to or greater than that of resin beads can be obtained, thus completing the present invention.
すなわち、本発明によれば、無機材料を主体とする基材粉体の表面の少なくとも一部を、カチオン界面活性剤及びアミノ変性シリコーンで表面処理することにより、カチオン界面活性剤及びアミノ変性シリコーンで表面処理された無機材料を主体とする基材粉体からなる複合表面処理無機粉体が提供される。That is, according to the present invention, by surface-treating at least a portion of the surface of a base powder mainly made of an inorganic material with a cationic surfactant and an amino-modified silicone, a composite surface-treated inorganic powder is provided, which is made of a base powder mainly made of an inorganic material and surface-treated with a cationic surfactant and an amino-modified silicone.
本発明により得られた複合表面処理無機粉体は、樹脂ビーズと同等又はそれ以上の肌への付着性と、使用時の肌への優れた感触を有しており、さらに化粧料に配合した場合は樹脂ビーズと同等又はそれ以上の感触を化粧料に付与することができる。The composite surface-treated inorganic powder obtained by the present invention has adhesion to the skin equal to or greater than that of resin beads and has an excellent feel on the skin when used, and further, when incorporated into cosmetics, it can impart to the cosmetics a feel equal to or greater than that of resin beads.
本発明の複合表面処理無機粉体は、基材として無機材料を主体とする基材粉体に特殊な複合表面処理を施しているので、そのような表面処理を施さない無機粉体に比べて平均粒子変形率が20%以上、より好ましくは23%以上という極めて柔らかな特性を有している。また、そのような平均粒子変形率を達成する基材粉体としては、シリカ、酸化チタン、酸化亜鉛、アルミナ及び酸化鉄からなる群から選択される1種又は2種以上を含むものが挙げられる。The composite surface-treated inorganic powder of the present invention has a special composite surface treatment applied to a base powder mainly made of an inorganic material as a base material, and therefore has extremely soft characteristics with an average particle deformation rate of 20% or more, more preferably 23% or more, compared to inorganic powders that have not been subjected to such surface treatment. In addition, examples of base powders that achieve such an average particle deformation rate include those containing one or more types selected from the group consisting of silica, titanium oxide, zinc oxide, alumina, and iron oxide.
本発明の複合表面処理無機粉体は、表面処理剤の1つとしてカチオン界面活性剤を使用することにより、樹脂ビーズと同等又はそれ以上の肌への付着性と、使用時の肌への優れた感触特性を得ることができる。 By using a cationic surfactant as one of the surface treatment agents, the composite surface-treated inorganic powder of the present invention can obtain adhesion to the skin equal to or greater than that of resin beads, as well as excellent tactile properties on the skin during use.
表面処理剤として使用できるカチオン界面活性剤の種類は特に限定されないが、上記特性を得るためには、炭素数が8から26の長鎖アルキル基を有する第4級アンモニウム塩を使用することが好ましい。この中でも、長鎖アルキル基を2つ有するものがより好ましい。There are no particular limitations on the type of cationic surfactant that can be used as a surface treatment agent, but in order to obtain the above characteristics, it is preferable to use a quaternary ammonium salt having a long-chain alkyl group with 8 to 26 carbon atoms. Among these, those having two long-chain alkyl groups are more preferable.
使用できるカチオン界面活性剤の具体例としては、例えば塩化ジステアリルジメチルアンモニウム、塩化ジアルキル(C12-C18)ジメチルアンモニウム、塩化ラウリルトリメチルアンモニウム、塩化ステアリルトリメチルアンモニウム、塩化セチルトリメチルアンモニウム、塩化オクタデシロキシプロピルトリメチルアンモニウム、塩化ベヘニルトリメチルアンモニウム、塩化ベンザルコニウムなどを挙げることができ、この中でも、塩化ジステアリルジメチルアンモニウムを使用することが特に好ましい。 Specific examples of cationic surfactants that can be used include distearyl dimethyl ammonium chloride, dialkyl (C12-C18) dimethyl ammonium chloride, lauryl trimethyl ammonium chloride, stearyl trimethyl ammonium chloride, cetyl trimethyl ammonium chloride, octadecyloxypropyl trimethyl ammonium chloride, behenyl trimethyl ammonium chloride, and benzalkonium chloride. Of these, it is particularly preferable to use distearyl dimethyl ammonium chloride.
カチオン界面活性剤の表面処理量は、基材粉体100質量部に対して0.1~5.0質量部であることが好ましく、0.1~2.0質量部であることがより好ましい。このような範囲の処理量で表面処理を施すことによって、さらに使用時の感触が良好な複合表面処理無機粉体を得ることができる。また、表面処理量が少な過ぎる場合は、肌への付着性が良好でなく、塗布後の化粧料が落ち易くなる場合がある。一方、表面処理量が多過ぎる場合は、肌に塗布した際にべたつく等、感触面での不都合を生じる場合がある。なお、本願明細書において「~」を用いて示された数値(比率)範囲は、「~」の前後に記載される数値(比率)をそれぞれ最小値(比率)及び最大値(比率)として含む範囲を示している。The surface treatment amount of the cationic surfactant is preferably 0.1 to 5.0 parts by mass, more preferably 0.1 to 2.0 parts by mass, per 100 parts by mass of the base powder. By carrying out the surface treatment with a treatment amount in this range, a composite surface-treated inorganic powder with a better feel during use can be obtained. Furthermore, if the surface treatment amount is too small, the adhesion to the skin may be poor and the cosmetic may easily come off after application. On the other hand, if the surface treatment amount is too large, it may cause inconvenience in terms of feel, such as stickiness when applied to the skin. In addition, the numerical value (ratio) range indicated using "~" in this specification indicates a range that includes the numerical values (ratios) written before and after "~" as the minimum value (ratio) and maximum value (ratio), respectively.
本発明の複合表面処理無機粉体は、表面処理剤の他の1つとしてアミノ変性シリコーンを使用することにより、樹脂ビーズと同等又はそれ以上の柔らかい感触を得ることができる。 The composite surface-treated inorganic powder of the present invention can achieve a soft feel equal to or even softer than that of resin beads by using amino-modified silicone as another surface treatment agent.
アミノ変性シリコーンの表面処理量は、基材粉体100質量部に対して0.5~5.0質量部であることが好ましく、0.5~2.0質量部であることがより好ましい。このような範囲の処理量で表面処理を施すことによって、複合表面処理無機粉体の感触を非常に良好なものにすることができる。表面処理量が少な過ぎる場合は、肌への塗布時に基材である無機材料特有の固さを感じ易く、感触が劣る場合がある。一方、表面処理量が多過ぎる場合は、肌への塗布時にべたつきを感じるなど、やはり感触が劣る場合がある。The amount of amino-modified silicone used for surface treatment is preferably 0.5 to 5.0 parts by mass, and more preferably 0.5 to 2.0 parts by mass, per 100 parts by mass of base powder. By carrying out surface treatment with a treatment amount in this range, the feel of the composite surface-treated inorganic powder can be made very good. If the amount of surface treatment is too small, the hardness specific to the inorganic material used as the base material may be easily felt when applied to the skin, and the feel may be poor. On the other hand, if the amount of surface treatment is too large, the feel may also be poor, such as a sticky feeling when applied to the skin.
また、本発明の複合表面処理無機粉体を配合すれば、樹脂ビーズを配合したのと同等又はそれ以上の柔らかさ、しっとり感やさらさら感といった使用感を発現する油性分散体や化粧料を得ることができる。 Furthermore, by incorporating the composite surface-treated inorganic powder of the present invention, it is possible to obtain oil-based dispersions and cosmetics that exhibit a feel when used that is equal to or greater than that when resin beads are incorporated, such as softness, moistness, and smoothness.
本発明によれば、無機材料を主体とする基材粉体の表面の少なくとも一部を、カチオン界面活性剤及びアミノ変性シリコーンで表面処理することにより、カチオン界面活性剤及びアミノ変性シリコーンで表面処理された無機材料を主体とする基材粉体からなる複合表面処理無機粉体が提供される。According to the present invention, at least a portion of the surface of a base powder mainly made of an inorganic material is surface-treated with a cationic surfactant and an amino-modified silicone to provide a composite surface-treated inorganic powder consisting of a base powder mainly made of an inorganic material that has been surface-treated with a cationic surfactant and an amino-modified silicone.
その結果、本発明によれば、シリカなどの無機材料を基材としながら、有機物質である樹脂ビーズと同等又はそれ以上の柔らかさを有しており、かつ肌への付着性に優れた複合表面処理無機粉体を得ることができる。As a result, according to the present invention, it is possible to obtain a composite surface-treated inorganic powder that uses an inorganic material such as silica as a base material, but has softness equal to or greater than that of resin beads, which are organic substances, and has excellent adhesion to the skin.
また、本発明によれば、本発明の複合表面処理無機粉体を配合することにより、樹脂ビーズを配合したのと同等又はそれ以上の柔らかさ、しっとり感やさらさら感といった使用感を発現する油性分散体や化粧料を得ることができる。 In addition, according to the present invention, by blending the composite surface-treated inorganic powder of the present invention, it is possible to obtain an oil-based dispersion or cosmetic that exhibits a feeling of use such as softness, moistness, and smoothness equivalent to or greater than that achieved by blending resin beads.
以下、本発明の複合表面処理無機粉体及びその製造方法、その無機粉体が配合されている油性分散体及び化粧料について具体例を交えながら詳細に説明する。なお、本発明は以下に示される実施形態に限定されるものではなく、本発明の技術的思想を逸脱しない範囲内で各種の変更が可能である。The composite surface-treated inorganic powder of the present invention, its manufacturing method, and the oil dispersion and cosmetic composition containing the inorganic powder will be described in detail below, with specific examples. Note that the present invention is not limited to the embodiments shown below, and various modifications are possible within the scope of the technical concept of the present invention.
(基材粉体)
本発明の複合表面処理無機粉体の基材として使用可能な無機材料は特に制限されず、例えばシリカ、酸化チタン、酸化亜鉛、アルミナ、酸化鉄などを使用することができる。この中でも、特にシリカが好ましい。
(Base Powder)
There are no particular limitations on the inorganic material that can be used as the base material of the composite surface-treated inorganic powder of the present invention, and examples of the inorganic material that can be used include silica, titanium oxide, zinc oxide, alumina, iron oxide, etc. Among these, silica is particularly preferred.
また、基材粉体は、レーザー回折光散乱法で測定される平均粒子径が、0.1~50μmの範囲であるものが好ましく、0.3~30μmの範囲のものがより好ましく、1~15μmの範囲ものが更に好ましい。平均粒子径が0.1μmより小さいと、粒子同士が凝集し易いことによって均一な表面処理がなされず、感触が向上し難い場合があり、50μmより大きいと物理的なざらつき感が強くなる場合がある。なお、後述の実施例では、基材粉体をメタノールに添加し、1分間超音波照射して分散させたのち、粒子径分布測定装置(マイクロトラック・ベル社製:マイクロトラックHRA)を用いて、平均粒子径を測定した。 The base powder preferably has an average particle size measured by a laser diffraction light scattering method in the range of 0.1 to 50 μm, more preferably in the range of 0.3 to 30 μm, and even more preferably in the range of 1 to 15 μm. If the average particle size is smaller than 0.1 μm, the particles tend to aggregate with each other, which may prevent uniform surface treatment and make it difficult to improve the feel, and if it is larger than 50 μm, the physical roughness may become stronger. In the examples described below, the base powder was added to methanol and dispersed by ultrasonic irradiation for 1 minute, and then the average particle size was measured using a particle size distribution measuring device (Microtrac HRA manufactured by Microtrac-Bell).
さらに、基材粉体の粒子形状は、通常化粧料に用いられるものであれば、球状、略球状、半球状、紡錘状、針状、板状、多面体状、星型状などいずれの形状でも良いが、球状、略球状、半球状などの丸みのある形状が好ましい。また、基材粉体の粒子は、無孔質、多孔質のいずれでもよい。 Furthermore, the particle shape of the base powder may be any shape commonly used in cosmetics, such as spherical, approximately spherical, hemispherical, spindle-shaped, needle-shaped, plate-shaped, polyhedral, or star-shaped, but rounded shapes such as spherical, approximately spherical, or hemispherical are preferred. The particles of the base powder may be either nonporous or porous.
(カチオン界面活性剤)
本発明の複合表面処理無機粉体において、表面処理剤としてカチオン界面活性剤を使用することで、肌への付着性が良好な、使用時の感触に優れる複合表面処理無機粉体を得ることができる。
(Cationic Surfactant)
In the composite surface-treated inorganic powder of the present invention, by using a cationic surfactant as the surface treatment agent, it is possible to obtain a composite surface-treated inorganic powder that has good adhesion to the skin and is excellent in feel during use.
表面処理剤として使用できるカチオン界面活性剤の種類は特に限定されないが、炭素数が8から26の長鎖アルキル基を有する第4級アンモニウム塩を使用することが好ましい。この中でも、長鎖アルキル基を2つ有するものがより好ましい。There are no particular limitations on the type of cationic surfactant that can be used as a surface treatment agent, but it is preferable to use a quaternary ammonium salt having a long-chain alkyl group with a carbon number of 8 to 26. Among these, those having two long-chain alkyl groups are more preferable.
使用できるカチオン界面活性剤の具体例として、塩化ジステアリルジメチルアンモニウム、塩化ジアルキル(C12-C18)ジメチルアンモニウム、塩化ラウリルトリメチルアンモニウム、塩化ステアリルトリメチルアンモニウム、塩化セチルトリメチルアンモニウム、塩化オクタデシロキシプロピルトリメチルアンモニウム、塩化ベヘニルトリメチルアンモニウム、塩化ベンザルコニウムなどが挙げられる。この中でも、塩化ジステアリルジメチルアンモニウムを使用することが特に好ましい。 Specific examples of cationic surfactants that can be used include distearyl dimethyl ammonium chloride, dialkyl (C12-C18) dimethyl ammonium chloride, lauryl trimethyl ammonium chloride, stearyl trimethyl ammonium chloride, cetyl trimethyl ammonium chloride, octadecyloxypropyl trimethyl ammonium chloride, behenyl trimethyl ammonium chloride, benzalkonium chloride, etc. Among these, it is particularly preferable to use distearyl dimethyl ammonium chloride.
カチオン界面活性剤の表面処理量は、基材粉体100質量部に対して0.1~5.0質量部であることが好ましく、0.1~2.0質量部であることがより好ましい。このような範囲の処理量で表面処理を施すことによって、さらに使用時の感触が良好な複合表面処理無機粉体を得ることができる。また、表面処理量が少な過ぎる場合は、肌への付着性が良好でなく、塗布後の化粧料が落ち易くなる場合がある。一方、表面処理量が多過ぎる場合は、肌に塗布した際にべたつく等、感触面での不都合を生じる場合がある。The surface treatment amount of the cationic surfactant is preferably 0.1 to 5.0 parts by mass, and more preferably 0.1 to 2.0 parts by mass, per 100 parts by mass of the base powder. By carrying out the surface treatment with a treatment amount in this range, it is possible to obtain a composite surface-treated inorganic powder that has an even better feel when used. Furthermore, if the surface treatment amount is too small, the adhesion to the skin may be poor and the cosmetic may easily come off after application. On the other hand, if the surface treatment amount is too large, it may cause inconvenience in terms of feel, such as stickiness when applied to the skin.
(アミノ変性シリコーン)
本発明の複合表面処理無機粉体において、表面処理剤としてアミノ変性シリコーンを使用することで、複合表面処理無機粉体に柔らかい感触を付与することができる。
(Amino modified silicone)
In the composite surface-treated inorganic powder of the present invention, by using an amino-modified silicone as a surface treatment agent, it is possible to impart a soft feel to the composite surface-treated inorganic powder.
表面処理剤として使用できるアミノ変性シリコーンの市販品の例として、信越化学工業社製のKF-8004、KF-8005S、KF-8015、KF-867S、X-52-2265、X-52-2328、ダウ・東レ社のDOWSIL(登録商標) SM8904Cosmetic Emulsion、SF8452C、SS-3551、ワッカー・ケミー社製のBELSIL(登録商標) ADM1370、ADM1650、ADM8103E、ADM8104E、ADM8105E、ADM9700E、ADM6300E、ADM6057E、ADM8301E、ADM6102E、ADM9000E、モメンティブ・パフォーマンス・マテリアルズ社のXF42-B1989、XF42-B8922、XF42-C0330、SF1708、XF49-C1109、Silsoft(登録商標) AX、Silsoft A+などが挙げられる。Examples of commercially available amino-modified silicones that can be used as surface treatment agents include Shin-Etsu Chemical's KF-8004, KF-8005S, KF-8015, KF-867S, X-52-2265, and X-52-2328; Dow-Toray's DOWSIL (registered trademark) SM8904 Cosmetic Emulsion, SF8452C, and SS-3551; and Wacker Chemie's BELSIL (registered trademark). Examples of such materials include ADM1370, ADM1650, ADM8103E, ADM8104E, ADM8105E, ADM9700E, ADM6300E, ADM6057E, ADM8301E, ADM6102E, ADM9000E, Momentive Performance Materials' XF42-B1989, XF42-B8922, XF42-C0330, SF1708, XF49-C1109, Silsoft (registered trademark) AX, and Silsoft A+.
アミノ変性シリコーンの表面処理量は、基材粉体100質量部に対して0.5~5.0質量部であることが好ましく、0.5~2.0質量部であることがより好ましい。このような範囲の処理量で表面処理を施すことによって、複合表面処理無機粉体の感触を非常に良好なものにすることができる。表面処理量が少な過ぎる場合は、肌への塗布時に基材である無機材料特有の固さを感じ易く、感触が劣る場合がある。一方、表面処理量が多過ぎる場合は、肌への塗布時にべたつきを感じるなど、やはり感触が劣る場合がある。The amount of amino-modified silicone used for surface treatment is preferably 0.5 to 5.0 parts by mass, and more preferably 0.5 to 2.0 parts by mass, per 100 parts by mass of base powder. By carrying out surface treatment with a treatment amount in this range, the feel of the composite surface-treated inorganic powder can be made very good. If the amount of surface treatment is too small, the hardness specific to the inorganic material used as the base material may be easily felt when applied to the skin, and the feel may be poor. On the other hand, if the amount of surface treatment is too large, the feel may also be poor, such as a sticky feeling when applied to the skin.
(表面処理方法)
本発明の複合表面処理無機粉体を得るための表面処理方法は、基材粉体や表面処理剤の物性を考慮して適宜選択すればよい。例えば、基材粉体を分散媒に分散させ、表面処理剤を添加して撹拌したのち、ろ過、乾燥する方法でもよいし、乾燥状態の粉体に表面処理剤を添加して混合する方法でもよく、これらに限定されない。なお、カチオン界面活性剤で表面処理を行う際には、水を含む分散媒を用いることが好ましい。
(Surface treatment method)
The surface treatment method for obtaining the composite surface-treated inorganic powder of the present invention may be appropriately selected in consideration of the physical properties of the base powder and the surface treatment agent. For example, the base powder may be dispersed in a dispersion medium, the surface treatment agent may be added and stirred, and then the mixture may be filtered and dried, or the surface treatment agent may be added to the dry powder and mixed, but is not limited thereto. When performing surface treatment with a cationic surfactant, it is preferable to use a dispersion medium containing water.
(平均粒子変形率)
本発明の複合表面処理無機粉体は、以下の方法で得られる平均粒子変形率が20%以上、より好ましくは23%以上であることが好ましい。このような平均粒子変形率を付与することで、表面処理を施さない無機粉体に比べて極めて柔らかな特性を備え、そして優れた感触を有する複合表面処理無機粉体とすることができる。
(Average particle deformation ratio)
The composite surface-treated inorganic powder of the present invention preferably has an average particle deformation ratio of 20% or more, more preferably 23% or more, obtained by the following method. By imparting such an average particle deformation ratio, it is possible to obtain a composite surface-treated inorganic powder that has extremely soft properties and an excellent feel compared to inorganic powders that have not been surface-treated.
(平均粒子変形率の算出方法)
平均粒子変形率を算出するための測定は、JIS Z8844(微小粒子の破壊強度及び変形強度の測定方法)に記載された方法に準じて行う。
まず、複合表面処理無機粉体から粒子をランダムにサンプリングし、試料台にセットする。
次に、圧子の先端を試料粒子に接触させた状態で、試料台と圧子の間の距離を測定し、これを試料粒子の粒子径D(μm)とする。
次に、試験力(粒子を圧子で圧縮するときに加える力)を5mNとして試料粒子を圧縮し、そのときの変位X(μm)を測定する。
変位X(μm)と、試料粒子の粒子径D(μm)から、以下の式に基づいて、試料粒子の粒子変形率を算出する。
式:粒子変形率(%)=変位X(μm)/試料粒子の粒子径D(μm)×100
この測定を5個の試料粒子に対して行い、得られる粒子変形率の平均値を平均粒子変形率とする。
(Method of calculating average particle deformation ratio)
The measurement for calculating the average particle deformation ratio is carried out in accordance with the method described in JIS Z8844 (Method for measuring the breaking strength and deformation strength of fine particles).
First, particles are randomly sampled from the composite surface-treated inorganic powder and set on a sample stage.
Next, with the tip of the indenter in contact with the sample particle, the distance between the sample stage and the indenter is measured, and this is taken as the particle diameter D (μm) of the sample particle.
Next, the sample particle is compressed with a test force (force applied when compressing the particle with an indenter) of 5 mN, and the displacement X (μm) at this time is measured.
The particle deformation rate of the sample particle is calculated from the displacement X (μm) and the particle diameter D (μm) of the sample particle according to the following formula.
Formula: Particle deformation rate (%) = displacement X (μm) / particle diameter D (μm) of sample particle × 100
This measurement is carried out for five sample particles, and the average value of the obtained particle deformation ratios is regarded as the average particle deformation ratio.
(化粧料)
本発明の複合表面処理無機粉体をファンデーションなどの化粧料に配合することにより、或いは本発明の複合表面処理無機粉体を油性分散体に配合し、前記油性分散体をファンデーションなどの化粧料に配合することにより、使用時の感触が優れた化粧料を得ることができる。
(Cosmetics)
By incorporating the composite surface-treated inorganic powder of the present invention into a cosmetic such as a foundation, or by incorporating the composite surface-treated inorganic powder of the present invention into an oil dispersion and then incorporating the oil dispersion into a cosmetic such as a foundation, a cosmetic having an excellent feel when used can be obtained.
1.化粧料用粉体の作製
(実施例1)
<工程1:カチオン界面活性剤での表面処理>
平均粒子径が5μmであるシリカ粉体(AGCエスアイテック社製:サンスフェアNP-30)100gをイオン交換水1000gに分散し、80℃に加熱後、濃度75質量%の塩化ジステアリルジメチルアンモニウム(日光ケミカルズ社製:NIKKOL CA-3475V)1.3gを投入して60分間撹拌し、ろ過、水洗後、乾燥機に入れて85℃で20時間乾燥させた。なお、日光ケミカルズ社製:NIKKOL CA-3475Vは、濃度75質量%の塩化ジステアリルジメチルアンモニウムである。
<工程2:アミノ変性シリコーンでの表面処理>
工程1で得られた粉体を卓上ブレンダーに入れ、そこにアミノ変性シリコーン(信越化学工業社製:KF-8004)2.0gを投入して20分間撹拌し、乾燥機に入れて120℃で3時間乾燥したのち、粉砕を行うことで、実施例1の複合表面処理無機粉体を作製した。 1. Preparation of cosmetic powder (Example 1)
<Step 1: Surface treatment with cationic surfactant>
100 g of silica powder (Sunsphere NP-30, manufactured by AGC Si-Tech Co., Ltd.) having an average particle size of 5 μm was dispersed in 1000 g of ion-exchanged water, and the mixture was heated to 80° C., after which 1.3 g of distearyldimethylammonium chloride having a concentration of 75% by mass (NIKKOL CA-3475V, manufactured by Nikko Chemicals Co., Ltd.) was added and stirred for 60 minutes, filtered, washed with water, and then placed in a dryer and dried at 85° C. for 20 hours. Note that NIKKOL CA-3475V, manufactured by Nikko Chemicals Co., Ltd., is distearyldimethylammonium chloride having a concentration of 75% by mass.
<Step 2: Surface treatment with amino-modified silicone>
The powder obtained in step 1 was placed in a benchtop blender, and 2.0 g of amino-modified silicone (KF-8004, manufactured by Shin-Etsu Chemical Co., Ltd.) was added thereto and stirred for 20 minutes. The mixture was then placed in a dryer and dried at 120°C for 3 hours, and then pulverized to produce the composite surface-treated inorganic powder of Example 1.
(実施例2)
塩化ジステアリルジメチルアンモニウムの投入量を0.13gとした以外は、実施例1と同様の操作を行って実施例2の複合表面処理無機粉体を作製した。
Example 2
A composite surface-treated inorganic powder of Example 2 was prepared by carrying out the same procedure as in Example 1, except that the amount of distearyldimethylammonium chloride added was 0.13 g.
(実施例3)
塩化ジステアリルジメチルアンモニウムの投入量を0.65gとした以外は、実施例1と同様の操作を行って実施例3の複合表面処理無機粉体を作製した。
Example 3
A composite surface-treated inorganic powder of Example 3 was prepared by carrying out the same procedure as in Example 1, except that the amount of distearyldimethylammonium chloride added was 0.65 g.
(実施例4)
塩化ジステアリルジメチルアンモニウムの投入量を2.6gとした以外は、実施例1と同様の操作を行って実施例4の複合表面処理無機粉体を作製した。
Example 4
A composite surface-treated inorganic powder of Example 4 was prepared by carrying out the same procedure as in Example 1, except that the amount of distearyldimethylammonium chloride added was 2.6 g.
(実施例5)
アミノ変性シリコーンの投入量を0.5gとした以外は、実施例1と同様の操作を行って実施例5の複合表面処理無機粉体を作製した。
Example 5
A composite surface-treated inorganic powder of Example 5 was prepared by carrying out the same procedure as in Example 1, except that the amount of amino-modified silicone added was 0.5 g.
(実施例6)
アミノ変性シリコーンの投入量を1.0gとした以外は、実施例1と同様の操作を行って実施例6の複合表面処理無機粉体を作製した。
Example 6
A composite surface-treated inorganic powder of Example 6 was prepared by carrying out the same procedure as in Example 1, except that the amount of amino-modified silicone added was 1.0 g.
(実施例7)
アミノ変性シリコーンの投入量を5.0gとした以外は、実施例1と同様の操作を行って実施例7の複合表面処理無機粉体を作製した。
(Example 7)
A composite surface-treated inorganic powder of Example 7 was prepared by carrying out the same procedure as in Example 1, except that the amount of amino-modified silicone added was 5.0 g.
(実施例8)
平均粒子径が3μmであるシリカ粉体(鈴木油脂工業社製:ゴッドボールG-6C)を使用した以外は、実施例1と同様の操作を行って実施例8の複合表面処理無機粉体を作製した。
(Example 8)
The composite surface-treated inorganic powder of Example 8 was prepared by the same procedure as in Example 1, except that silica powder having an average particle size of 3 μm (Godball G-6C, manufactured by Suzuki Oil Industries Co., Ltd.) was used.
(実施例9)
平均粒子径が10μmであるシリカ粉体(AGCエスアイテック社製:サンスフェアNP-100)を使用した以外は、実施例1と同様の操作を行って実施例9の複合表面処理無機粉体を作製した。
Example 9
The composite surface-treated inorganic powder of Example 9 was prepared by the same procedure as in Example 1, except that silica powder having an average particle size of 10 μm (Sunsphere NP-100, manufactured by AGC Si-Tech Co., Ltd.) was used.
(比較例1)
実施例1の複合表面処理無機粉体の基材であるシリカ粉体(AGCエスアイテック社製:サンスフェアNP-30)を、比較例1の粉体とした。
(Comparative Example 1)
The silica powder (Sunsphere NP-30, manufactured by AGC Si-Tech Co., Ltd.), which is the base material of the composite surface-treated inorganic powder of Example 1, was used as the powder of Comparative Example 1.
(比較例2)
平均粒子径が5μmであるシリカ粉体(AGCエスアイテック社製:サンスフェアNP-30)100gを卓上ブレンダーに入れ、そこにジメチコン(信越化学工業社製:KF-96-1000CS)2.0gを投入して20分間撹拌し、乾燥機に入れて120℃で3時間乾燥したのち、粉砕を行うことで、比較例2の粉体を作製した。
(Comparative Example 2)
100 g of silica powder (Sunsphere NP-30, manufactured by AGC Si-Tech Co., Ltd.) having an average particle size of 5 μm was placed in a benchtop blender, 2.0 g of dimethicone (KF-96-1000CS, manufactured by Shin-Etsu Chemical Co., Ltd.) was added thereto, and the mixture was stirred for 20 minutes. The mixture was then placed in a dryer and dried at 120° C. for 3 hours, and then pulverized to produce the powder of Comparative Example 2.
(比較例3)
実施例1の工程1のみを行うことにより得られた粉体を、比較例3の粉体とした。
(Comparative Example 3)
The powder obtained by carrying out only step 1 of Example 1 was used as the powder of Comparative Example 3.
(比較例4)
実施例1の工程1で得られた粉体の代わりに、実施例1の複合表面処理無機粉体の基材であるシリカ粉体(AGCエスアイテック社製:サンスフェアNP-30)を使用して、実施例1の工程2のみを行うことにより、比較例4の粉体を作製した。
(Comparative Example 4)
Instead of the powder obtained in step 1 of Example 1, silica powder (Sunsphere NP-30 manufactured by AGC Si-Tech Co., Ltd.), which is the base material of the composite surface-treated inorganic powder of Example 1, was used, and only step 2 of Example 1 was carried out to produce the powder of Comparative Example 4.
(参考例1)
シリコーン樹脂ビーズ(モメンティブ・パフォーマンス・マテリアルズ社製:トスパール(登録商標)145A)を、参考例1の粉体とした。
(Reference Example 1)
Silicone resin beads (Tospearl (registered trademark) 145A, manufactured by Momentive Performance Materials, Inc.) were used as the powder in Reference Example 1.
(平均粒子変形率の算出)
実施例、比較例、参考例の各粉体からランダムでサンプリングした5個の試料粒子について、微小粒子圧壊力測定装置(ナノシーズ社製:NS-A100)を使用して、粒子径D(μm)と、試験力5mNで圧縮したときの変位X(μm)を測定し、以下の式から得られる粒子変形率を平均することによって、各粉体の平均粒子変形率を算出した。
粒子変形率(%)=変位X(μm)/試料粒子の粒子径D(μm)×100
(Calculation of average particle deformation ratio)
For five sample particles randomly sampled from each powder in the Examples, Comparative Examples, and Reference Examples, a microparticle crushing force measuring device (NS-A100 manufactured by Nano Seeds Corporation) was used to measure the particle diameter D (μm) and the displacement X (μm) when compressed with a test force of 5 mN. The particle deformation ratios obtained from the following formula were averaged to calculate the average particle deformation ratio of each powder.
Particle deformation rate (%) = displacement X (μm) / particle diameter D (μm) of sample particle × 100
(各粉体の肌への付着性及び感触の評価)
実施例、比較例、参考例の各粉体について、モニター5人の官能試験によって、肌への付着性及び感触の評価を行った。具体的には、各粉体を少量取って手の甲に指で塗布した際の、肌への付着性及び感触を、以下の基準で評価してもらい、その平均値を算出することにより行った。
<評価点の基準>
5点:非常に優れている
4点:優れている
3点:普通
2点:劣る
1点:非常に劣る
(Evaluation of adhesion and feel of each powder to the skin)
Each powder of the Examples, Comparative Examples, and Reference Examples was evaluated for its adhesion to the skin and its feel by a sensory test conducted by five monitors. Specifically, a small amount of each powder was taken and applied to the back of the hand with the fingers, and the monitors were asked to evaluate the adhesion to the skin and its feel according to the following criteria, and the average value was calculated.
<Evaluation criteria>
5 points: Very good 4 points: Good 3 points: Average 2 points: Poor 1 point: Very bad
実施例、比較例、参考例の各粉体の作製条件及び評価結果(平均粒子変形率、肌への付着性、感触)を表1に示す。
表1より、実施例1~9の複合表面処理無機粉体は、樹脂ビーズである参考例1の粉体(シリコーン樹脂)と同等又はそれ以上の肌への付着性と、使用時の肌への優れた感触特性を得ることができることが判った。一方、比較例1~4の粉体は、少なくとも肌への付着性又は感触のいずれかが劣る結果であった。 From Table 1, it can be seen that the composite surface-treated inorganic powders of Examples 1 to 9 have adhesion to the skin equal to or greater than that of the powder (silicone resin) of Reference Example 1, which is a resin bead, and provide excellent feel characteristics on the skin during use. On the other hand, the powders of Comparative Examples 1 to 4 were inferior in at least either adhesion to the skin or feel.
また、実施例1~9の複合表面処理無機粉体は、表面処理を施さなかった比較例1の無機粉体、カチオン界面活性剤及びアミノ変性シリコーン以外の表面処理剤(ジメチコン)による表面処理を施した比較例2の無機粉体、カチオン界面活性剤による表面処理のみ施した比較例3の無機粉体及びアミノ変性シリコーンによる表面処理のみ施した比較例3の無機粉体よりも優れた肌への付着性と、使用時の肌への優れた感触特性を得られるのみならず、平均粒子変形率においても20%以上、より好ましくは23%以上という極めて柔らかな特性を有していることが判った。このため、一般的に硬いとされるシリカなどの無機粉体において、上述のような特性を得るためには、表面処理剤として塩化ジステアリルジメチルアンモニウムなどのカチオン界面活性剤及びアミノ変性シリコーンを用いることが極めて有効であることが判った。 In addition, the composite surface-treated inorganic powders of Examples 1 to 9 not only have superior adhesion to the skin and superior feel to the skin during use compared to the inorganic powder of Comparative Example 1, which was not surface-treated, the inorganic powder of Comparative Example 2, which was surface-treated with a surface treatment agent other than a cationic surfactant and amino-modified silicone (dimethicone), the inorganic powder of Comparative Example 3, which was surface-treated only with a cationic surfactant, and the inorganic powder of Comparative Example 3, which was surface-treated only with an amino-modified silicone, but also have extremely soft characteristics, with an average particle deformation rate of 20% or more, more preferably 23% or more. Therefore, in order to obtain the above-mentioned characteristics in inorganic powders such as silica, which are generally considered to be hard, it has been found that it is extremely effective to use a cationic surfactant such as distearyldimethylammonium chloride and an amino-modified silicone as a surface treatment agent.
また、実施例1~9の複合表面処理無機粉体と比較例1~4の粉体との比較により、カチオン界面活性剤の表面処理量は、基材粉体100質量部に対して0.1~5.0質量部、更には0.1~2.0質量部であることが好ましく、アミノ変性シリコーンの表面処理量は、基材粉体100質量部に対して0.5~5.0質量部、更には0.5~2.0質量部であることが好ましいことが判った。Furthermore, by comparing the composite surface-treated inorganic powders of Examples 1 to 9 with the powders of Comparative Examples 1 to 4, it was found that the surface treatment amount of the cationic surfactant is preferably 0.1 to 5.0 parts by mass, and more preferably 0.1 to 2.0 parts by mass, per 100 parts by mass of the base powder, and the surface treatment amount of the amino-modified silicone is preferably 0.5 to 5.0 parts by mass, and more preferably 0.5 to 2.0 parts by mass, per 100 parts by mass of the base powder.
また、実施例1~9の複合表面処理無機粉体は、レーザー回折光散乱法で測定される平均粒子径が好ましくは0.1~50μmの範囲、より好ましくは0.3~30μmの範囲、更に好ましくは1~15μmの範囲以内であると、粒子同士の凝集によって均一な表面処理が阻害されず、感触が向上し、物理的なざらつき感も抑制されることが判った。In addition, it was found that when the composite surface-treated inorganic powders of Examples 1 to 9 have an average particle size measured by a laser diffraction light scattering method within the range of preferably 0.1 to 50 μm, more preferably 0.3 to 30 μm, and even more preferably 1 to 15 μm, uniform surface treatment is not hindered by aggregation of particles, the feel is improved, and the physical roughness is suppressed.
2.化粧料の作製
次に、表2に示す配合組成(質量部)で実施例10、比較例5、参考例2の化粧料(W/Oサンスクリーンミルク:SPF50+、PA++++)を作製した。具体的には、化粧料の油相を構成する各材料を混合した油性組成物(油性分散体)と、化粧料の水相を構成する各材料を混合した水性組成物を作製したのち、これらを混合することにより作製した。 2. Preparation of Cosmetics Next, cosmetics (W/O sunscreen milk: SPF50+, PA++++) of Example 10, Comparative Example 5, and Reference Example 2 were prepared with the blending compositions (parts by mass) shown in Table 2. Specifically, an oily composition (oil-based dispersion) was prepared by mixing the materials constituting the oil phase of the cosmetics, and an aqueous composition was prepared by mixing the materials constituting the aqueous phase of the cosmetics, and then these were mixed to prepare the cosmetics.
(各化粧料の感触の評価)
得られた各化粧料について、モニター10人の官能試験によって使用感の評価を行った。具体的には、各化粧料の塗布量が2mg/cm2となるように前腕の内側に塗布した際の、柔らかさ、滑らかさ、きしみの無さを、以下の基準で評価してもらい、その平均値を算出することにより行った。
<評価点の基準>
5点:非常に優れている
4点:優れている
3点:普通
2点:劣る
1点:非常に劣る
(Evaluation of the feel of each cosmetic)
The obtained cosmetics were subjected to a sensory test by 10 monitors to evaluate the feel of use. Specifically, each cosmetic was applied to the inside of the forearm in an amount of 2 mg/ cm2, and the monitors were asked to evaluate the softness, smoothness, and absence of squeaking according to the following criteria, and the average value was calculated.
<Evaluation criteria>
5 points: Very good 4 points: Good 3 points: Average 2 points: Poor 1 point: Very bad
実施例10、比較例5、参考例2の化粧料の配合組成及び評価結果(柔らかさ、滑らかさ、きしみの無さ)を表2に示す。
表2より、実施例10の化粧料は、実施例1の複合表面処理無機粉体を配合したことにより、樹脂ビーズである参考例1の粉体(シリコーン樹脂)を配合した参考例2の化粧料よりも優れた使用感(柔らかさ、滑らかさ、きしみの無さ)を得ることができることが判った。一方、比較例1の粉体を配合した比較例5の化粧料は、特に柔らかさやきしみの無さにおいて、実施例10の化粧料よりも使用感が劣る結果であった。 From Table 2, it was found that the cosmetic of Example 10, which contains the composite surface-treated inorganic powder of Example 1, provides a better feel (softness, smoothness, and lack of squeaking) than the cosmetic of Reference Example 2, which contains the powder of Reference Example 1 (silicone resin), which is a resin bead. On the other hand, the cosmetic of Comparative Example 5, which contains the powder of Comparative Example 1, provided an inferior feel to the cosmetic of Example 10, particularly in terms of softness and lack of squeaking.
次に、表3に示す配合組成(質量部)で実施例11、比較例6、参考例3の粉体化粧料(フェイスパウダー)を作製し、前述の化粧料(W/Oサンスクリーンミルク)の方法と同様にして、使用感の評価を行った。Next, powder cosmetics (face powder) of Example 11, Comparative Example 6, and Reference Example 3 were prepared with the formulation (parts by weight) shown in Table 3, and the sensation of use was evaluated in the same manner as for the aforementioned cosmetic (W/O sunscreen milk).
実施例11、比較例6、参考例3の粉体化粧料の配合及び評価結果(柔らかさ、滑らかさ、きしみの無さ)を表3に示す。
表3より、実施例11の粉体化粧料は、実施例1の複合表面処理無機粉体を配合したことにより、樹脂ビーズである参考例1の粉体(シリコーン樹脂)を配合した参考例3の化粧料と同等以上の使用感(柔らかさ、滑らかさ、きしみの無さ)を得ることができることが判った。一方、比較例6の化粧料は、特に柔らかさにおいて、実施例11の化粧料よりも使用感が大きく劣る結果であった。
From Table 3, it was found that the powder cosmetic of Example 11, by blending the composite surface-treated inorganic powder of Example 1, was able to obtain a feel in use (softness, smoothness, absence of squeaking) equal to or better than that of the cosmetic of Reference Example 3, which blended the powder (silicone resin) of Reference Example 1, which is resin beads. On the other hand, the cosmetic of Comparative Example 6 resulted in a feel in use that was significantly inferior to that of Example 11, particularly in terms of softness.
Claims (10)
前記基材粉体はシリカであり、
前記カチオン界面活性剤は、塩化ジステアリルジメチルアンモニウム、塩化ジアルキル(C12-C18)ジメチルアンモニウム、塩化ラウリルトリメチルアンモニウム、塩化ステアリルトリメチルアンモニウム、塩化セチルトリメチルアンモニウム、塩化オクタデシロキシプロピルトリメチルアンモニウム、塩化ベヘニルトリメチルアンモニウム及び塩化ベンザルコニウムからなる群から選択される1種又は2種以上を含み、
前記カチオン界面活性剤の表面処理量は、前記基材粉体100質量部に対して0.1~5.0質量部であり、
前記アミノ変性シリコーンの表面処理量は、前記基材粉体100質量部に対して0.5~5.0質量部である、化粧料に配合される複合表面処理無機粉体。 A base powder mainly made of an inorganic material is surface-treated with a cationic surfactant and an amino-modified silicone,
The base powder is silica,
The cationic surfactant includes one or more selected from the group consisting of distearyl dimethyl ammonium chloride, dialkyl (C12-C18) dimethyl ammonium chloride, lauryl trimethyl ammonium chloride, stearyl trimethyl ammonium chloride, cetyl trimethyl ammonium chloride, octadecyloxypropyl trimethyl ammonium chloride, behenyl trimethyl ammonium chloride, and benzalkonium chloride;
The surface treatment amount of the cationic surfactant is 0.1 to 5.0 parts by mass relative to 100 parts by mass of the base powder,
The composite surface-treated inorganic powder to be blended in a cosmetic composition has a surface treatment amount of 0.5 to 5.0 parts by mass per 100 parts by mass of the base powder .
前記基材粉体はシリカであり、
前記カチオン界面活性剤は、塩化ジステアリルジメチルアンモニウム、塩化ジアルキル(C12-C18)ジメチルアンモニウム、塩化ラウリルトリメチルアンモニウム、塩化ステアリルトリメチルアンモニウム、塩化セチルトリメチルアンモニウム、塩化オクタデシロキシプロピルトリメチルアンモニウム、塩化ベヘニルトリメチルアンモニウム及び塩化ベンザルコニウムからなる群から選択される1種又は2種以上を含み、
前記カチオン界面活性剤の表面処理量は、前記基材粉体100質量部に対して0.1~5.0質量部であり、
前記アミノ変性シリコーンの表面処理量は、前記基材粉体100質量部に対して0.5~5.0質量部である、化粧料に配合される複合表面処理無機粉体の製造方法。 The method includes surface-treating at least a portion of a surface of a base powder mainly made of an inorganic material with a cationic surfactant and an amino-modified silicone,
The base powder is silica,
The cationic surfactant includes one or more selected from the group consisting of distearyl dimethyl ammonium chloride, dialkyl (C12-C18) dimethyl ammonium chloride, lauryl trimethyl ammonium chloride, stearyl trimethyl ammonium chloride, cetyl trimethyl ammonium chloride, octadecyloxypropyl trimethyl ammonium chloride, behenyl trimethyl ammonium chloride, and benzalkonium chloride;
The surface treatment amount of the cationic surfactant is 0.1 to 5.0 parts by mass relative to 100 parts by mass of the base powder,
The method for producing a composite surface-treated inorganic powder to be blended in a cosmetic, wherein the surface treatment amount of the amino-modified silicone is 0.5 to 5.0 parts by mass per 100 parts by mass of the base powder .
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| WO2007077673A1 (en) | 2005-12-28 | 2007-07-12 | Agc Si-Teck Co., Ltd. | Water-repellent inorganic powder and process for production thereof |
| WO2014102862A1 (en) | 2012-12-26 | 2014-07-03 | 三好化成株式会社 | Surface-treated powder and cosmetic containing same |
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| JP2002173611A (en) | 2000-12-05 | 2002-06-21 | Maruo Calcium Co Ltd | Surface modified inorganic particles and coating composition containing the particles |
| WO2007077673A1 (en) | 2005-12-28 | 2007-07-12 | Agc Si-Teck Co., Ltd. | Water-repellent inorganic powder and process for production thereof |
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