JP4505211B2 - Method for producing surface-treated powder, amino-modified silicone-treated powder and cosmetic - Google Patents
Method for producing surface-treated powder, amino-modified silicone-treated powder and cosmetic Download PDFInfo
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- JP4505211B2 JP4505211B2 JP2003390160A JP2003390160A JP4505211B2 JP 4505211 B2 JP4505211 B2 JP 4505211B2 JP 2003390160 A JP2003390160 A JP 2003390160A JP 2003390160 A JP2003390160 A JP 2003390160A JP 4505211 B2 JP4505211 B2 JP 4505211B2
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- 239000000843 powder Substances 0.000 title claims description 50
- 239000002537 cosmetic Substances 0.000 title claims description 27
- 229920001296 polysiloxane Polymers 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 238000011282 treatment Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 230000000052 comparative effect Effects 0.000 description 14
- -1 methyl hydrogen Chemical compound 0.000 description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 8
- 230000006835 compression Effects 0.000 description 8
- 238000007906 compression Methods 0.000 description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000000454 talc Substances 0.000 description 7
- 229910052623 talc Inorganic materials 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000049 pigment Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000010445 mica Substances 0.000 description 5
- 229910052618 mica group Inorganic materials 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 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
- 229940073609 bismuth oxychloride Drugs 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000012756 surface treatment agent Substances 0.000 description 2
- XLTMWFMRJZDFFD-UHFFFAOYSA-N 1-[(2-chloro-4-nitrophenyl)diazenyl]naphthalen-2-ol Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C([N+]([O-])=O)C=C1Cl XLTMWFMRJZDFFD-UHFFFAOYSA-N 0.000 description 1
- GNCOVOVCHIHPHP-UHFFFAOYSA-N 2-[[4-[4-[(1-anilino-1,3-dioxobutan-2-yl)diazenyl]-3-chlorophenyl]-2-chlorophenyl]diazenyl]-3-oxo-n-phenylbutanamide Chemical compound C=1C=CC=CC=1NC(=O)C(C(=O)C)N=NC(C(=C1)Cl)=CC=C1C(C=C1Cl)=CC=C1N=NC(C(C)=O)C(=O)NC1=CC=CC=C1 GNCOVOVCHIHPHP-UHFFFAOYSA-N 0.000 description 1
- UBVSIAHUTXHQTD-UHFFFAOYSA-N 2-n-(4-bromophenyl)-1,3,5-triazine-2,4-diamine Chemical compound NC1=NC=NC(NC=2C=CC(Br)=CC=2)=N1 UBVSIAHUTXHQTD-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 description 1
- 235000004936 Bromus mango Nutrition 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 240000007228 Mangifera indica Species 0.000 description 1
- 235000014826 Mangifera indica Nutrition 0.000 description 1
- 239000004909 Moisturizer Substances 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 235000009184 Spondias indica Nutrition 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229940121363 anti-inflammatory agent Drugs 0.000 description 1
- 239000002260 anti-inflammatory agent Substances 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 229940064004 antiseptic throat preparations Drugs 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 239000003212 astringent agent Substances 0.000 description 1
- IRERQBUNZFJFGC-UHFFFAOYSA-L azure blue Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[S-]S[S-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] IRERQBUNZFJFGC-UHFFFAOYSA-L 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052916 barium silicate Inorganic materials 0.000 description 1
- POJOORKDYOPQLS-UHFFFAOYSA-L barium(2+) 5-chloro-2-[(2-hydroxynaphthalen-1-yl)diazenyl]-4-methylbenzenesulfonate Chemical compound [Ba+2].C1=C(Cl)C(C)=CC(N=NC=2C3=CC=CC=C3C=CC=2O)=C1S([O-])(=O)=O.C1=C(Cl)C(C)=CC(N=NC=2C3=CC=CC=C3C=CC=2O)=C1S([O-])(=O)=O POJOORKDYOPQLS-UHFFFAOYSA-L 0.000 description 1
- HMOQPOVBDRFNIU-UHFFFAOYSA-N barium(2+);dioxido(oxo)silane Chemical compound [Ba+2].[O-][Si]([O-])=O HMOQPOVBDRFNIU-UHFFFAOYSA-N 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 229910052626 biotite Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- HBHZKFOUIUMKHV-UHFFFAOYSA-N chembl1982121 Chemical compound OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O HBHZKFOUIUMKHV-UHFFFAOYSA-N 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- VQWFNAGFNGABOH-UHFFFAOYSA-K chromium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Cr+3] VQWFNAGFNGABOH-UHFFFAOYSA-K 0.000 description 1
- 229910000152 cobalt phosphate Inorganic materials 0.000 description 1
- LFSBSHDDAGNCTM-UHFFFAOYSA-N cobalt(2+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Co+2] LFSBSHDDAGNCTM-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 1
- LQJVOKWHGUAUHK-UHFFFAOYSA-L disodium 5-amino-4-hydroxy-3-phenyldiazenylnaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].OC1=C2C(N)=CC(S([O-])(=O)=O)=CC2=CC(S([O-])(=O)=O)=C1N=NC1=CC=CC=C1 LQJVOKWHGUAUHK-UHFFFAOYSA-L 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000012732 erythrosine Nutrition 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- SXQCTESRRZBPHJ-UHFFFAOYSA-M lissamine rhodamine Chemical compound [Na+].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=C(S([O-])(=O)=O)C=C1S([O-])(=O)=O SXQCTESRRZBPHJ-UHFFFAOYSA-M 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 230000001333 moisturizer Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052627 muscovite Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000007764 o/w emulsion Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 229910052628 phlogopite Inorganic materials 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052917 strontium silicate Inorganic materials 0.000 description 1
- QSQXISIULMTHLV-UHFFFAOYSA-N strontium;dioxido(oxo)silane Chemical compound [Sr+2].[O-][Si]([O-])=O QSQXISIULMTHLV-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- OTMNKCRTGBGNPN-UHFFFAOYSA-N sulfanylidenebarium Chemical compound [Ba]=S OTMNKCRTGBGNPN-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- UJMBCXLDXJUMFB-UHFFFAOYSA-K trisodium;5-oxo-1-(4-sulfonatophenyl)-4-[(4-sulfonatophenyl)diazenyl]-4h-pyrazole-3-carboxylate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)C1=NN(C=2C=CC(=CC=2)S([O-])(=O)=O)C(=O)C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 UJMBCXLDXJUMFB-UHFFFAOYSA-K 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000007762 w/o emulsion Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Description
本発明は、化粧品に配合でき、撥水性、伸展性、付着性、感触、打型成型性に優れたアミノ変性シリコーン処理粉体、およびその製造方法に関する。 The present invention relates to an amino-modified silicone-treated powder that can be blended in cosmetics and has excellent water repellency, extensibility, adhesion, feel, and moldability, and a method for producing the same.
メチルハイドロジェンポリシロキサン（メチコン）等のシリコーンならびにシラン剤で表面処理を行ったタルク、マイカ、セリサイト等が、ファンデーション等の化粧品原料として数多く市販されている。これらの表面処理は、撥水性、ならびに表面の滑沢性向上を目的として行われており、現在、従来から知られているメチコン処理により概ね目的が達成されていると考えられているが、その製造面から考えた場合、従来の技術によるメチコン処理では、処理粉体が二次凝集を起こしやすく、また処理粉体に水素が残留する場合がある等の問題があった。 Many talc, mica, sericite, and the like surface-treated with silicone such as methyl hydrogen polysiloxane (methicone) and silane agent are commercially available as cosmetic raw materials such as foundations. These surface treatments are performed for the purpose of improving water repellency and surface lubricity, and it is considered that the purpose is generally achieved by the conventionally known methicone treatment. From the viewpoint of manufacturing, the methicone treatment according to the conventional technique has problems such as that the treated powder tends to cause secondary agglomeration and hydrogen may remain in the treated powder.
そこで、従来技術によるメチコン処理の残留水素の問題を解決するために、分子鎖末端にアミノ水素基、アルコキシ基等を有する直鎖状反応性アルキルポリシロキサンを表面処理剤として使用することが提案されている（特許文献１）。 Therefore, in order to solve the problem of residual hydrogen in the methicone treatment according to the prior art, it has been proposed to use a linear reactive alkylpolysiloxane having an amino hydrogen group, an alkoxy group or the like at the molecular chain end as a surface treatment agent. (Patent Document 1).
特許文献１では、処理にあたり、上記直鎖状反応性アルキルポリシロキサン、顔料、有機溶媒等を混合し、１０５℃以上の高温条件下における加熱処理により、均一な表面処理を成し遂げているが、高温加熱処理では処理剤が変性してしまう可能性があり、また粉体同士の結合力が弱い為、打型成形性が劣り化粧料に対するバインダーの配合量が多くなり、製品の感触に悪い影響を与えている。 In Patent Document 1, the above-mentioned linear reactive alkylpolysiloxane, pigment, organic solvent, etc. are mixed for the treatment, and a uniform surface treatment is achieved by heat treatment under a high temperature condition of 105 ° C. or higher. In the heat treatment, the treatment agent may be denatured, and since the bonding force between the powders is weak, the moldability is inferior and the amount of binder added to the cosmetic is increased, which adversely affects the feel of the product. Giving.
以上の通り、従来の技術によるメチコン処理、あるいは特許文献１で提案されている処理では、化粧品配合用の処理粉体としての性能は未だ満足のいくものではなかった。化粧品原料としての優劣は、官能試験による感触等によって決められることが多く、感触がメチコン処理や高温加熱処理に優る新規処理粉体が望まれていた。
本発明の目的は、従来技術の問題を解決するためになされたもので、非常にしっとりとした感触を持ち、伸展性、付着性、打型成型性、撥水性に優れた表面処理粉体およびその製造方法を提供することにある。 The object of the present invention was made to solve the problems of the prior art, has a very moist feel, and is a surface-treated powder excellent in extensibility, adhesion, moldability, and water repellency. It is in providing the manufacturing method.
本発明者らは上記目的達成のため鋭意研究を重ねた結果、アミノ変性シリコーンをずり剪断式低速混練機で粉体に処理する方法が極めて有効であることを見出し、本発明を完成するに至った。 As a result of intensive studies to achieve the above object, the present inventors have found that a method for treating amino-modified silicone with a low-speed kneader using a shearing shearing method is extremely effective, and completed the present invention. It was.
即ち、本発明は、ずり剪断式低速混練機を用い、粉体表面をアミノ変性シリコーンで処理することを特徴とする表面処理粉体の製造方法であって、本発明ではアミノ変性シリコーンを母材となる粉体の０．１〜１０重量％添加し、メカノケミカル的混合技術の応用によるずり剪断式低速混練機を用いて、粉体粒子表面にアミノ変性シリコーンを擦りこむように、均一に万遍なく処理することで、従来にはないソフトでクリーミィな感触で伸展性、付着性、感触、打型成型性、撥水性に優れた化粧品原料となる表面処理粉体を得ることができる。 That is, the present invention is a method for producing a surface-treated powder, characterized in that the surface of the powder is treated with amino-modified silicone using a shear-shear type low-speed kneader, wherein the amino-modified silicone is used as a base material in the present invention. Add 0.1 to 10% by weight of the resulting powder, and use a shear-shearing low-speed kneader by applying mechanochemical mixing technology to uniformly rub amino-modified silicone onto the powder particle surface. By performing the treatment without any treatment, it is possible to obtain a surface-treated powder that is a raw material for cosmetics that has a soft, creamy feel that is not conventional and has excellent extensibility, adhesion, feel, moldability, and water repellency.
さらに本発明によれば、本発明の上記処理粉体を化粧料の一成分もしくは全成分に用いた場合、バインダーの配合割合の低いもしくはバインダーを必要としない固形粉体化粧料が提供される。 Furthermore, according to the present invention, when the above-mentioned treated powder of the present invention is used as one component or all components of a cosmetic, a solid powder cosmetic having a low blending ratio of the binder or requiring no binder is provided.
本発明の表面処理粉体の製造方法は、ずり剪断式低速混練機を用いることにより常温での処理を可能とし、この処理粉体を用いることにより従来の撥水性を保持しながら、より打型性に優れ、伸展性、付着性、しっとり感が良好な化粧品を得ることができる。このように優れた性質を有する処理方法及び処理粉体は、粉体化粧料、固形粉体化粧料、液状化粧料、油性化粧料等に配合することにより、化粧料の品質向上に著しく貢献する。 The method for producing the surface-treated powder of the present invention enables processing at room temperature by using a shear shear type low-speed kneader, and by using this treated powder, while maintaining the conventional water repellency, it is more moldable. It is possible to obtain a cosmetic product having excellent properties and excellent extensibility, adhesion and moist feeling. The treatment method and the treated powder having such excellent properties significantly contribute to the improvement of the quality of the cosmetic by being blended with the powder cosmetic, the solid powder cosmetic, the liquid cosmetic, the oily cosmetic, and the like. .
以下に本発明を詳述する。本発明で用いる処理装置は、表面処理剤と母剤となる粉体とをメカノケミカル的混合技術を応用して、ずり剪断式混練により常温で処理することができる低速混練機であれば良い。このような混練機としては、雷潰機、ニーダー（特殊機化株式会社、大野化学機械株式会社、株式会社ダルトン他）、ミックスマラー（新東工業株式会社）、ＧＳミル（株式会社マキノ）および石臼等が挙げられる。尚、ここで言う常温での処理とは、加熱処理は意図しないという意味であり、常温とは２５℃前後であって、敢えて規定すれば２０〜３０℃程度を意味する。 The present invention is described in detail below. The processing apparatus used in the present invention may be any low-speed kneader that can treat the surface treatment agent and the powder serving as a base material at room temperature by shear shear kneading by applying a mechanochemical mixing technique. Such kneaders include thunder crushers, kneaders (special mechanization Co., Ltd., Ohno Chemical Machinery Co., Ltd., Dalton Co., Ltd.), mix muller (Shinto Kogyo Co., Ltd.), GS mill (Makino Co., Ltd.) and Examples include stone mortars. In addition, the treatment at normal temperature mentioned here means that heat treatment is not intended, and normal temperature means around 25 ° C., which means about 20 to 30 ° C. if it is deliberately defined.
また、アミノ変性シリコーンを母材となる粉体への配合量（被覆量）は、０．１〜１０重量％（好ましくは２〜６重量％）である。また、具体的処理方法としては、アミノ変性シリコーンと粉体とを数時間かけて混練し、粉体表面をアミノ変性シリコーンで被覆処理する方法である。 Further, the blending amount (covering amount) of the amino-modified silicone into the powder as a base material is 0.1 to 10% by weight (preferably 2 to 6% by weight). As a specific treatment method, amino-modified silicone and powder are kneaded over several hours, and the powder surface is coated with amino-modified silicone.
本発明で用いられる装置は、ずり剪断式であることが必須条件であり、通常の高速混合機（ヘンシェルミキサー等）を用いた場合、処理は可能であるがずり剪断式装置ほど優良な効果を得るには至らなかった。 It is essential that the apparatus used in the present invention is a shear shear type. When an ordinary high-speed mixer (Henschel mixer or the like) is used, the processing is possible, but the shear shear type apparatus has a better effect. I didn't get it.
例えば、アミノ変性シリコーンを処理剤とした他の表面処理方法としては、ヘンシェルミキサー、スーパーミキサー等の乾式高速混合機を用いて、母剤となる粉体に対して２〜５重量％量程度のシリコーン処理剤を２〜１０重量％量程度の溶媒と共に均一に混合後、低温乾燥を行うことで、感触等の優良化を試みることが考えられるが、このような方法ではシリコーン処理剤の粉体への密着が不十分となる。 For example, as another surface treatment method using amino-modified silicone as a treatment agent, a dry high-speed mixer such as a Henschel mixer or a supermixer is used, and the amount is about 2 to 5% by weight with respect to the base powder. It is conceivable to try to improve the feeling by touching the silicone treating agent uniformly with a solvent of about 2 to 10% by weight and then drying at low temperature. Adhesion to the is insufficient.
次に、本発明の表面処理剤として使われるアミノ変性シリコーンとは、ポリシロキサンの側鎖および／または末端に有機基を持つ反応性シリコーンオイルの一種であり、例えば下記構造式（１）で表されるアミノプロピルメチルシロキサン・ジメチルシロキサン共重合体等を挙げることができる。 Next, the amino-modified silicone used as the surface treating agent of the present invention is a kind of reactive silicone oil having an organic group at the side chain and / or terminal of polysiloxane, and is represented by the following structural formula (1), for example. And aminopropylmethylsiloxane / dimethylsiloxane copolymer.
（式中、ｍは５０〜３００の整数、ｎは１〜１０の整数である。）
また、アミノ変性シリコーンで処理される母剤となる粉体、および化粧料において本発明による表面処理粉体以外に必要に応じて加えられる粉体は、通常化粧料として用いられるものであれば特に限定されず、例えば、タルク、白雲母、合成雲母、金雲母、紅雲母、黒雲母、リチア雲母、セリサイト、カオリン、二酸化チタン等の体質顔料、酸化チタン被覆雲母、酸化チタン被覆タルク、酸化チタン被覆オキシ塩化ビスマス、オキシ塩化ビスマス、魚鱗箔、着色酸化チタン被覆雲母等のパール顔料、アルミニウムパウダー、酸化鉄（ベンガラ）、黄酸化鉄、黒酸化鉄、カーボンブラック、マンゴバイオレット、コバルトバイオレット、酸化クロム、水酸化クロム、チタン酸コバルト、群青、紺青等の無機着色顔料、亜鉛華、ベントナイト、硫酸バリウム、金属石鹸、珪ソウ土、ケイ酸アルミニウム、ケイ酸カルシウム、ケイ酸バリウム、ケイ酸マグネシウム、ケイ酸ストロンチウム、タングステン酸金属塩、炭酸カルシウム、炭酸マグネシウム、アルミナ、ヒドロキシアパタイト、窒化ホウ素、シリカ、ナイロンパウダー、ゼオライト、ポリエチレンパウダー、ポリスチレンパウダー、セルロースパウダー、シリコーン樹脂粉末等の無機・有機顔料、赤色３号、赤色１０４号、赤色１０６号、赤色２０１号、赤色２０２号、赤色２０４号、赤色２０５号、赤色２２０号、赤色２２６号、赤色２２７号、赤色２２８号、赤色２３０号、赤色４０１号、赤色４０５号、赤色５０５号、だいだい色２０３号、だいだい色２０４号、だいだい色２０５号、黄色４号、黄色５号、黄色２０２号、黄色２０３号、黄色２０５号、黄色４０１号、青色１号、青色４０４号、緑色３号及びジルコニウム、バリウムまたはアルミニウムレーキ等のタール系色素、フッ素処理粉体、無機粉体被覆顔料等表面処理粉体などである。
(In the formula, m is an integer of 50 to 300, and n is an integer of 1 to 10.)
In addition, the powder used as a base material to be treated with amino-modified silicone, and the powder to be added as necessary in addition to the surface-treated powder according to the present invention in the cosmetic are particularly those that are usually used as cosmetics. For example, body pigments such as talc, muscovite, synthetic mica, phlogopite, red mica, biotite, lithia mica, sericite, kaolin, titanium dioxide, titanium oxide coated mica, titanium oxide coated talc, titanium oxide Coated bismuth oxychloride, bismuth oxychloride, fish scale foil, colored titanium oxide coated pearl pigments such as mica, aluminum powder, iron oxide (Bengara), yellow iron oxide, black iron oxide, carbon black, mango violet, cobalt violet, chromium oxide , Inorganic color pigments such as chromium hydroxide, cobalt titanate, ultramarine and bitumen, zinc white, bentonite, sulfur Barium, metal soap, siliceous earth, aluminum silicate, calcium silicate, barium silicate, magnesium silicate, strontium silicate, metal tungstate, calcium carbonate, magnesium carbonate, alumina, hydroxyapatite, boron nitride, silica, Inorganic / organic pigments such as nylon powder, zeolite, polyethylene powder, polystyrene powder, cellulose powder, silicone resin powder, red No. 3, red No. 104, red No. 106, red No. 201, red No. 202, red No. 204, red 205 No., Red No. 220, Red No. 226, Red No. 227, Red No. 228, Red No. 230, Red No. 401, Red No. 405, Red No. 505, Orange No. 203, No. Color No. 204, No. Color No. 205, Yellow No. 4, Yellow No. 5, Yellow No. 202 Yellow No. 203, Yellow No. 205, Yellow No. 401, Blue No. 1, Blue No. 404, Green No. 3, and tar-based pigments such as zirconium, barium or aluminum lake, fluorine-treated powders, surface-treated powders such as inorganic powder-coated pigments Such as the body.
上記アミノ変性シリコーン処理粉体は化粧料として好適に使用される。この場合、油性成分、保湿剤、紫外線吸収剤、酸化防止剤、防腐剤、消炎剤、ビタミン、ホルモンなどの薬剤、香料、ｐＨ調整剤、金属封鎖剤、収斂剤等の通常化粧品に配合される他の成分を配合することは勿論可能である。 The amino-modified silicone-treated powder is suitably used as a cosmetic. In this case, it is blended in conventional cosmetics such as oily ingredients, moisturizers, UV absorbers, antioxidants, antiseptics, anti-inflammatory agents, vitamins, hormones, etc., perfumes, pH adjusters, sequestering agents, astringents, etc. Of course, it is possible to mix | blend another component.
また、当然のことながら、精製水および水溶性成分および適切な界面活性剤を配合して液状化粧料としたり、乳化技術を駆使することによって、油中水型あるいは水中油型の乳化組成物とすることも可能である。 Naturally, purified water, water-soluble components and an appropriate surfactant are blended into a liquid cosmetic, or by using an emulsification technique, a water-in-oil or oil-in-water emulsion composition and It is also possible to do.
以下、実施例によって本発明を更に詳細に説明するが、これは本発明を限定するものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this does not limit this invention.
尚、夫々の実施例、比較例について、打型製品の成形性、パフへの取れ、撥水性の観察を行った。結果を表２に示す。 In addition, about each Example and the comparative example, the moldability of the punching product, the removal to a puff, and water repellency were observed. The results are shown in Table 2.
また、実用特性の評価については、２０名の女性パネラーに試料を顔に塗布させ、肌への伸展性、付着性、感触について以下の評価基準で評価し、全員の平均値を算出した。結果を表４に示す。
（評価基準）
良い ４、やや良い ３、普通 ２、やや悪い １、悪い ０
実施例１ パウダーファンデーション（成形性）
表１の実施例１の成分配合量の通り、成分Ａを均一混合し、成分Ｂを加え、雷潰機にて３時間混合し、ハンマーミルで粉砕した後、これをアルミ皿に適量採り、圧縮成型した。
実施例２ パウダーファンデーション（成形性）
表１の実施例２の成分配合量の通り、成分Ａを均一混合し、成分Ｂを加え、雷潰機にて３時間混合し、ハンマーミルで粉砕した後、アルミ皿に適量採り、圧縮成型した。
比較例１
表1の比較例1の成分配合量の通り、成分Ａを均一混合し、成分Ｂを加え、高速混合機（ヘンシェルミキサー）にて１０分混合し、ハンマーミルで粉砕をした後、アルミ皿に適量採り、圧縮成型した。
比較例２
表１の比較例2の成分配合量の通り、成分Ａを均一混合し、成分Ｂを加え、高速混合機（ヘンシェルミキサー）で１０分混合した。次に１５０℃で３時間加熱処理をし、ハンマーミルで粉砕をした後、アルミ皿に適量採り、圧縮成型した。
比較例３
表１の比較例３の成分配合量の通り、成分Ａを均一混合し、成分Ｂを加え、雷潰機で３時間混合した。次に１５０℃で３時間加熱処理をし、ハンマーミルで粉砕をした後、アルミ皿に適量採り、圧縮成型した。
比較例４
表１の比較例４の成分配合量の通り、成分Ａを均一混合し、雷潰機にて３時間混合し、ハンマーミルで粉砕した後、アルミ皿に適量採り、圧縮成型した。
Regarding the evaluation of practical characteristics, samples were applied to 20 female panelists on the face, and the extensibility, adhesion, and feel to the skin were evaluated according to the following evaluation criteria, and the average value of all members was calculated. The results are shown in Table 4.
(Evaluation criteria)
Good 4, Slightly good 3, Normal 2, Slightly bad 1, Bad 0
Example 1 Powder foundation (formability)
According to the amount of component of Example 1 in Table 1, component A is uniformly mixed, component B is added, mixed for 3 hours with a thunder crusher, pulverized with a hammer mill, and an appropriate amount is taken in an aluminum dish. Compression molded.
Example 2 Powder foundation (formability)
As shown in Example 2 in Table 1, component A was mixed uniformly, component B was added, mixed for 3 hours with a thunder crusher, pulverized with a hammer mill, and then put in an appropriate amount in an aluminum dish and compression molded. did.
Comparative Example 1
As shown in Comparative Example 1 in Table 1, Component A is uniformly mixed, Component B is added, mixed for 10 minutes with a high-speed mixer (Henschel mixer), pulverized with a hammer mill, and then placed in an aluminum dish. An appropriate amount was taken and compression molded.
Comparative Example 2
According to the component blending amounts of Comparative Example 2 in Table 1, Component A was uniformly mixed, Component B was added, and mixed for 10 minutes with a high speed mixer (Henschel mixer). Next, after heat treatment at 150 ° C. for 3 hours and pulverization with a hammer mill, an appropriate amount was taken in an aluminum dish and compression molded.
Comparative Example 3
According to the compounding amount of Comparative Example 3 in Table 1, Component A was uniformly mixed, Component B was added, and the mixture was mixed for 3 hours with a thunder crusher. Next, after heat treatment at 150 ° C. for 3 hours and pulverization with a hammer mill, an appropriate amount was taken in an aluminum dish and compression molded.
Comparative Example 4
As shown in Comparative Example 4 in Table 1, Component A was uniformly mixed, mixed for 3 hours with a thunder crusher, pulverized with a hammer mill, and then taken into an aluminum dish and compression molded.
以上のように本発明のアミノ変性シリコーン処理は常温処理でありながら十分な撥水性を保持し、バインダーを配合せずに使用に耐えられる固形粉体化粧料が成型できた。また、高速混合機を用いるよりも成形性において良好な結果を得た（比較例１）。メチルハイドロジェンポリシロキサン処理粉体を用いた場合は高速混合機、ずり剪断式低速混練機のどちらを用いても、撥水性は有るものの本発明と同等の成形性を得ることが出来なかった（比較例２、３）。表面処理をしていない粉体では、成形性、撥水性どちらも劣っていた。（比較例4）
実施例３ パウダーファンデーション（実用特性）
タルク９５重量％とアミノプロピルメチルシロキサン・ジメチルシロキサン共重合体５重量％を雷潰機にて３時間混合し、ハンマーミルで粉砕してタルク５重量％アミノ変性シリコーン処理品を得た。同様にセリサイト、酸化チタンを処理し、セリサイト５重量％処理アミノ変性シリコーン処理品、酸化チタン５重量％アミノ変性シリコーン処理品を得た。
As described above, the amino-modified silicone treatment of the present invention was able to be molded into a solid powder cosmetic that can maintain a sufficient water repellency while being treated at room temperature and can be used without blending a binder. Also, better results were obtained in moldability than using a high-speed mixer (Comparative Example 1). When methylhydrogenpolysiloxane-treated powder was used, it was not possible to obtain formability equivalent to that of the present invention although water repellency was obtained using either a high speed mixer or a shear shear type low speed kneader ( Comparative examples 2 and 3). The powder not subjected to surface treatment was inferior in both moldability and water repellency. (Comparative Example 4)
Example 3 Powder foundation (practical properties)
95% by weight of talc and 5% by weight of aminopropylmethylsiloxane / dimethylsiloxane copolymer were mixed for 3 hours by a lightning machine and pulverized by a hammer mill to obtain a 5% by weight amino-modified silicone-treated product of talc. Similarly, sericite and titanium oxide were treated to obtain a sericite 5% by weight treated amino-modified silicone-treated product and a titanium oxide 5% by weight amino-modified silicone-treated product.
次に、表３の実施例3の成分配合量の通り、全成分を混合粉砕し、アルミ皿に適量採り、圧縮成型した。
比較例５
タルク９５重量％とメチルハイドロジェンポリシロキサン５重量％を高速混合機（ヘンシェルミキサー）で１０分混合した。次に１５０℃で３時間加熱処理をし、ハンマーミルで粉砕をしてタルク５重量％メチルハイドロジェンポリシロキサン処理品を得た。同様にセリサイト、酸化チタンを処理し、セリサイト５重量％メチルハイドロジェンポリシロキサン処理品、酸化チタン５重量％メチルハイドロジェンポリシロキサン処理品を得た。
Next, all the components were mixed and pulverized in accordance with the amounts of ingredients in Example 3 in Table 3, and an appropriate amount was taken in an aluminum dish and compression molded.
Comparative Example 5
95% by weight of talc and 5% by weight of methyl hydrogen polysiloxane were mixed with a high-speed mixer (Henschel mixer) for 10 minutes. Next, it was heat-treated at 150 ° C. for 3 hours and pulverized with a hammer mill to obtain a 5% by weight methylhydrogenpolysiloxane-treated product of talc. Similarly, sericite and titanium oxide were treated to obtain a sericite 5% by weight methylhydrogenpolysiloxane-treated product and a titanium oxide 5% by weight methylhydrogenpolysiloxane-treated product.
次に、表３の比較例5の成分配合量の通り、全成分を混合粉砕し、アルミ皿に適量採り、圧縮成型した。 Next, all the components were mixed and pulverized according to the compounding amounts of Comparative Example 5 in Table 3, taken in an appropriate amount in an aluminum dish, and compression molded.
以上のように本発明品を用いた固形粉体化粧料は、伸展性、付着性、感触（しっとり感）いずれにおいてもメチルハイドロジェンポリシロキサン処理品を用いた場合より良好な使用感を得た。 As described above, the solid powder cosmetic using the product of the present invention obtained a better feeling of use than the case of using the methylhydrogenpolysiloxane-treated product in any of extensibility, adhesion, and touch (moist feeling). .
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| JP5341333B2 (en) * | 2007-09-06 | 2013-11-13 | 株式会社 資生堂 | Method for producing powder cosmetics |
| KR20110133480A (en) * | 2009-03-18 | 2011-12-12 | 가부시키가이샤 시세이도 | Process for producing powdery composition and powdery cosmetic |
| JP6219603B2 (en) * | 2012-06-01 | 2017-10-25 | 株式会社コーセー | Solid powder cosmetic |
| JP6111444B2 (en) * | 2012-06-01 | 2017-04-12 | 株式会社コーセー | Powder cosmetics |
| JP6050061B2 (en) * | 2012-07-05 | 2016-12-21 | 株式会社コーセー | Powder cosmetics |
| JP6114066B2 (en) * | 2013-02-28 | 2017-04-12 | 株式会社コーセー | Solid powder cosmetic |
| KR102585843B1 (en) * | 2015-03-30 | 2023-10-11 | 가부시키가이샤 코세 | solid powder cosmetics |
| KR102332129B1 (en) | 2016-05-31 | 2021-11-29 | 가부시키가이샤 시세이도 | elastomer |
| JP7154007B2 (en) | 2017-11-28 | 2022-10-17 | 株式会社 資生堂 | emulsified cosmetic |
| KR20200138729A (en) | 2018-03-30 | 2020-12-10 | 가부시키가이샤 코세 | Phosphorylcholine group and silicone group-containing copolymer, powder coated with the copolymer and method for producing the same, and use of the copolymer and the powder as a cosmetic |
| JP7332352B2 (en) * | 2019-06-17 | 2023-08-23 | 株式会社ノエビア | Surface-treated powder and cosmetic containing surface-treated powder |
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| JPH0699266B2 (en) * | 1986-05-15 | 1994-12-07 | 株式会社資生堂 | Cosmetics |
| JP2739253B2 (en) * | 1990-08-22 | 1998-04-15 | 花王株式会社 | Cosmetics |
| JP3515282B2 (en) * | 1996-06-07 | 2004-04-05 | 京セラケミカル株式会社 | Electrostatic image developing toner and electrostatic image developing method |
| JPH11131048A (en) * | 1997-08-26 | 1999-05-18 | Kao Corp | Ultraviolet light screening complex fine particle |
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