JP6718742B2 - Hair dye - Google Patents
Hair dye Download PDFInfo
- Publication number
- JP6718742B2 JP6718742B2 JP2016105487A JP2016105487A JP6718742B2 JP 6718742 B2 JP6718742 B2 JP 6718742B2 JP 2016105487 A JP2016105487 A JP 2016105487A JP 2016105487 A JP2016105487 A JP 2016105487A JP 6718742 B2 JP6718742 B2 JP 6718742B2
- Authority
- JP
- Japan
- Prior art keywords
- hair
- dye
- silica
- hair dye
- mass
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired - Fee Related
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- 239000000118 hair dye Substances 0.000 title claims description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 79
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 238000004043 dyeing Methods 0.000 claims description 42
- 239000000377 silicon dioxide Substances 0.000 claims description 41
- 239000000049 pigment Substances 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 229920005989 resin Polymers 0.000 claims description 25
- 239000011347 resin Substances 0.000 claims description 25
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000980 acid dye Substances 0.000 claims description 16
- 239000002562 thickening agent Substances 0.000 claims description 15
- 239000006229 carbon black Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- 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 claims description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- 239000003002 pH adjusting agent Substances 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 claims description 2
- 238000011156 evaluation Methods 0.000 description 39
- 239000002245 particle Substances 0.000 description 21
- 230000001186 cumulative effect Effects 0.000 description 20
- 239000000975 dye Substances 0.000 description 19
- 239000011248 coating agent Substances 0.000 description 15
- 238000000576 coating method Methods 0.000 description 15
- -1 Yellow No. 4 Chemical compound 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 14
- 229920001897 terpolymer Polymers 0.000 description 11
- 238000004040 coloring Methods 0.000 description 10
- 238000001035 drying Methods 0.000 description 10
- 230000007794 irritation Effects 0.000 description 10
- 239000000178 monomer Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 235000013980 iron oxide Nutrition 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 230000002378 acidificating effect Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- SJEYSFABYSGQBG-UHFFFAOYSA-M Patent blue Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C(=CC(=CC=1)S([O-])(=O)=O)S([O-])(=O)=O)=C1C=CC(=[N+](CC)CC)C=C1 SJEYSFABYSGQBG-UHFFFAOYSA-M 0.000 description 4
- 229920000289 Polyquaternium Polymers 0.000 description 4
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 4
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 4
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 4
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 4
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 241000894007 species Species 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 244000007835 Cyamopsis tetragonoloba Species 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000001023 inorganic pigment Substances 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- OYINQIKIQCNQOX-UHFFFAOYSA-M 2-hydroxybutyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCC(O)C[N+](C)(C)C OYINQIKIQCNQOX-UHFFFAOYSA-M 0.000 description 2
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 description 2
- 241000283707 Capra Species 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 230000003020 moisturizing effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229920002050 silicone resin Polymers 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-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
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- FLCAEMBIQVZWIF-UHFFFAOYSA-N 6-(dimethylamino)-2-methylhex-2-enamide Chemical compound CN(C)CCCC=C(C)C(N)=O FLCAEMBIQVZWIF-UHFFFAOYSA-N 0.000 description 1
- MCPFORBUAZKAQE-UHFFFAOYSA-N 6-(dimethylamino)-2-methylhex-2-enoic acid Chemical compound CN(C)CCCC=C(C)C(O)=O MCPFORBUAZKAQE-UHFFFAOYSA-N 0.000 description 1
- WLDHEUZGFKACJH-ZRUFZDNISA-K Amaranth Chemical compound [Na+].[Na+].[Na+].C12=CC=C(S([O-])(=O)=O)C=C2C=C(S([O-])(=O)=O)C(O)=C1\N=N\C1=CC=C(S([O-])(=O)=O)C2=CC=CC=C12 WLDHEUZGFKACJH-ZRUFZDNISA-K 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- GDFCSMCGLZFNFY-UHFFFAOYSA-N Dimethylaminopropyl Methacrylamide Chemical compound CN(C)CCCNC(=O)C(C)=C GDFCSMCGLZFNFY-UHFFFAOYSA-N 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- CQPFMGBJSMSXLP-UHFFFAOYSA-M acid orange 7 Chemical compound [Na+].OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 CQPFMGBJSMSXLP-UHFFFAOYSA-M 0.000 description 1
- 229920006243 acrylic copolymer Polymers 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 239000001000 anthraquinone dye Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000000987 azo dye 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
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229920006317 cationic polymer Polymers 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
- MQWPIYMKAKYEEQ-UHFFFAOYSA-L dipotassium 2,3,4,5-tetrachloro-6-(2,4,5,7-tetrabromo-3-oxido-6-oxoxanthen-9-yl)benzoate Chemical compound [K+].[K+].[O-]C(=O)c1c(Cl)c(Cl)c(Cl)c(Cl)c1-c1c2cc(Br)c([O-])c(Br)c2oc2c(Br)c(=O)c(Br)cc12 MQWPIYMKAKYEEQ-UHFFFAOYSA-L 0.000 description 1
- VQHHOXOLUXRQFQ-UHFFFAOYSA-L dipotassium;4,5,6,7-tetrachloro-2',4',5',7'-tetraiodo-3-oxospiro[2-benzofuran-1,9'-xanthene]-3',6'-diolate Chemical compound [K+].[K+].O1C(=O)C(C(=C(Cl)C(Cl)=C2Cl)Cl)=C2C21C1=CC(I)=C([O-])C(I)=C1OC1=C(I)C([O-])=C(I)C=C21 VQHHOXOLUXRQFQ-UHFFFAOYSA-L 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
- FPAYXBWMYIMERV-UHFFFAOYSA-L disodium;5-methyl-2-[[4-(4-methyl-2-sulfonatoanilino)-9,10-dioxoanthracen-1-yl]amino]benzenesulfonate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)C1=CC(C)=CC=C1NC(C=1C(=O)C2=CC=CC=C2C(=O)C=11)=CC=C1NC1=CC=C(C)C=C1S([O-])(=O)=O FPAYXBWMYIMERV-UHFFFAOYSA-L 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000012732 erythrosine Nutrition 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 210000004517 glycocalyx Anatomy 0.000 description 1
- 230000037308 hair color Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000004356 hydroxy functional group Chemical group O* 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 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
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- JMXROTHPANUTOJ-UHFFFAOYSA-H naphthol green b Chemical compound [Na+].[Na+].[Na+].[Fe+3].C1=C(S([O-])(=O)=O)C=CC2=C(N=O)C([O-])=CC=C21.C1=C(S([O-])(=O)=O)C=CC2=C(N=O)C([O-])=CC=C21.C1=C(S([O-])(=O)=O)C=CC2=C(N=O)C([O-])=CC=C21 JMXROTHPANUTOJ-UHFFFAOYSA-H 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000001024 permanent hair color Substances 0.000 description 1
- 229960005323 phenoxyethanol Drugs 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 229940067107 phenylethyl alcohol Drugs 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 229940032159 propylene carbonate Drugs 0.000 description 1
- 229960004063 propylene glycol Drugs 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- KXXXUIKPSVVSAW-UHFFFAOYSA-K pyranine Chemical compound [Na+].[Na+].[Na+].C1=C2C(O)=CC(S([O-])(=O)=O)=C(C=C3)C2=C2C3=C(S([O-])(=O)=O)C=C(S([O-])(=O)=O)C2=C1 KXXXUIKPSVVSAW-UHFFFAOYSA-K 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- AZJPTIGZZTZIDR-UHFFFAOYSA-L rose bengal Chemical compound [K+].[K+].[O-]C(=O)C1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1C1=C2C=C(I)C(=O)C(I)=C2OC2=C(I)C([O-])=C(I)C=C21 AZJPTIGZZTZIDR-UHFFFAOYSA-L 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 210000004761 scalp Anatomy 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000001026 semi permanent hair color Substances 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- CGXSFOUXEQBDCJ-UHFFFAOYSA-N sodium;8-hydroxy-5,7-dinitronaphthalene-2-sulfonic acid Chemical compound [Na+].C1=C(S(O)(=O)=O)C=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 CGXSFOUXEQBDCJ-UHFFFAOYSA-N 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000001027 temporary hair color Substances 0.000 description 1
- 125000002088 tosyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1C([H])([H])[H])S(*)(=O)=O 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 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
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Landscapes
- Cosmetics (AREA)
Description
本発明は、耐水性に優れると共に、一時着色性に優れるだけでなく、使用する回数を重ねる毎に徐々に毛髪を染色していく累積染毛性にも優れる染毛料に関する。 The present invention relates to a hair dye which is excellent not only in water resistance but also in temporary coloring property, and is also excellent in cumulative hair dyeing property in which hair is gradually dyed with each repeated use.
従来より、一般的に汎用されている、永久染毛料(ヘアカラー、酸化染毛料)や半永久染毛料(ヘアマニキュア、酸性染毛料)は、使用時の染毛操作が複雑で、時間も要するだけでなく、周囲や衣服、被施術者の皮膚が染色されてしまうなどの大きな欠点を有している。
そのため、一般的には理美容室で施術してもらうか、若しくは入浴時に自己施術しなくてはならないなど、使用者への負担が大きいものであった。
Permanent hair dyes (hair colors, oxidative hair dyes) and semi-permanent hair dyes (hair manicure, acid hair dyes) that have been generally used conventionally are complicated in hair dyeing operation at the time of use and only take time. In addition, it has a big defect that the surroundings, clothes, and the skin of the subject are dyed.
Therefore, in general, it is a heavy burden on the user that he or she must be operated in a hairdressing salon or must be self-administered when taking a bath.
これらの負担を低減し、簡便に繰り返し使用することで累積的に染毛できる染毛料として、例えば、1)着色剤としての酸性染料を0.01〜3重量%、ノニオン若しくは
アニオンのシリコン系樹脂を0.1〜10重量%、染毛助剤を3〜20重量%、低級アルコールを30〜80重量%、水を5〜50重量%含有し、pHが2〜5、粘度が100mPa・s以下である累積染毛性一時染毛料及びその製造方法(例えば、特許文献1参照)、2)揮発性の低級アルコール40〜95重量%、増粘剤2〜10重量%、染毛助剤2〜30重量%、カーボンブラック、およびトリフェニルメタン染料、アゾ染料、キノリン染料、ザンセン染料、インジゴイド染料、アントラキノン染料のうち1種あるいは2種以上の染料を含み、pH値を1.5から4.5に調製してなることを特徴とする染毛用組成物(例えば、特許文献2参照)、3)水溶性染料の少なくとも1種0.4〜3重量%と、ノニオン若しくはアニオンのシリコーン系樹脂0.5〜7重量%と、カーボンブラック0.4〜4重量%と、アクリル系共重合体樹脂0.5〜6重量%と、低級アルコール15〜55重量%と、水20重量%以上とを含有し、かつ、pHを2〜5に調整してなることを特徴とする染毛料(例えば、特許文献3参照)が知られている。
As a hair dye that reduces these burdens and can be used for cumulative hair dyeing simply and repeatedly, for example, 1) 0.01 to 3% by weight of an acid dye as a colorant, a nonionic or anionic silicone resin 0.1 to 10% by weight, hair dyeing aid 3 to 20% by weight, lower alcohol 30 to 80% by weight, water 5 to 50% by weight, pH 2 to 5, viscosity 100 mPa·s. The following is a cumulative hair dyeing temporary hair dye and a method for producing the same (see, for example, Patent Document 1), 2) 40 to 95% by weight of a volatile lower alcohol, 2 to 10% by weight of a thickener, and a hair dyeing aid 2. .About.30% by weight, carbon black, and one or more dyes selected from triphenylmethane dye, azo dye, quinoline dye, zanthene dye, indigoid dye and anthraquinone dye, and having a pH value of 1.5 to 4. 5. A composition for hair dyeing, which is prepared in 5 (see, for example, Patent Document 2), 3) 0.4 to 3% by weight of at least one kind of water-soluble dye, and a nonionic or anionic silicone resin. 0.5 to 7% by weight, carbon black 0.4 to 4% by weight, acrylic copolymer resin 0.5 to 6% by weight, lower alcohol 15 to 55% by weight, and water 20% by weight or more There is known a hair dye (see, for example, Patent Document 3) that contains the above and has a pH adjusted to 2 to 5.
しかしながら、特許文献1の染毛料は優れた累積染毛性の染毛料となるものであるが、着色剤が酸性染料のみであり、白髪への一時着色性能がやや劣り、光源によっては、染めた部分が周囲の毛髪よりも若干明るく見えてしまうという課題が一部にあり、さらに、粘度が低いためにヘアマスカラなどの使用には不向きであった。
また、上記特許文献2の染毛料等は、塗布後の耐水性が得にくく、耐水性を向上させようとした場合、カーボンブラックの分散安定性が低下したり、酸性染料と凝集物を生じてしまう等、多くの課題がある。
また、上記特許文献3の染毛料は、優れた累積染毛性の染毛料となるものであるが、低pH環境下でカーボンブラックの色相が若干変化してしまい、一時着色時の色相と累積染毛時の色相に若干ズレが生じてしまうという課題が一部にあり、さらに、粘度が低いためにヘアマスカラなどの使用には不向きであった。
However, although the hair dye of Patent Document 1 is a hair dye with excellent cumulative hair dyeing properties, the coloring agent is only an acid dye, and the temporary coloring performance for white hair is slightly inferior, and depending on the light source, it is dyed. There is a problem in that the part looks a little brighter than the surrounding hair, and the low viscosity makes it unsuitable for use in hair mascaras.
Further, the hair dye or the like of the above-mentioned Patent Document 2 is difficult to obtain water resistance after application, and when it is attempted to improve water resistance, the dispersion stability of carbon black is lowered, or acid dyes and aggregates are generated. There are many problems such as being lost.
Further, although the hair dye of Patent Document 3 is a hair dye having excellent cumulative hair dyeing properties, the hue of carbon black is slightly changed in a low pH environment, and the hue and cumulative hue during temporary coloring are accumulated. There is a problem in that the hue during hair dyeing may be slightly deviated, and the low viscosity makes it unsuitable for use in hair mascaras.
本発明は、上記従来技術の課題等に鑑み、これを解消しようとするものであり、耐水性に優れると共に、低pH環境下でもシリカ被覆顔料を安定に分散でき、使用直後の洗髪が不要であり、塗布直後の毛髪染毛性に優れるだけでなく、使用する回数を重ねる毎に徐々に毛髪を染色していく累積染毛性、使用性に優れた染毛料を提供することを目的とする。 The present invention has been made in view of the above-mentioned problems of the prior art and is intended to solve this problem. In addition to being excellent in water resistance, the silica-coated pigment can be stably dispersed even in a low pH environment, and hair washing immediately after use is unnecessary. The present invention aims to provide a hair dye not only having excellent hair dyeability immediately after application, but also having a cumulative hair dyeing property that gradually dyes the hair each time it is used and an excellent usability. ..
本発明者らは、上記従来技術の課題等について鋭意検討を重ねた結果、酸性染料と、シリカ被覆顔料と、耐水性樹脂と、増粘剤とを少なくとも含み、粘度とpHをそれぞれ特定の範囲に調整することなどにより、上記目的の染毛料が得られることを見出し、本発明を完成させるに至ったのである。 As a result of intensive studies on the above-mentioned problems of the prior art, the present inventors have included at least an acid dye, a silica-coated pigment, a water resistant resin, and a thickener, and have a viscosity and a pH in specific ranges. It was found that the hair dye of the above-mentioned purpose can be obtained by adjusting the above to the present invention and completed the present invention.
すなわち、本発明は、次の(1)〜(3)に存する。
(1) 酸性染料の少なくとも1種0.1〜3質量%と、シリカ被覆顔料0.1〜10質量%と、耐水性樹脂0.5〜3質量%(固形分量)と、低級アルコール20〜60質量%と、染毛助剤2〜20質量%と、pH調整剤0.5〜10質量%と、増粘剤とを少なくとも含み、粘度が40〜200mPa・sであり、pHが2〜5に調整してなることを特徴とする染毛料。
(2) 前記シリカ被覆顔料は、黒酸化鉄、ベンガラ、黄酸化鉄、カーボンブラック、墨、酸化チタンから選ばれる少なくとも1種をシリカで表面処理されたものであることを特徴とする請求項1に記載の染毛料。
(3) 前記染毛料には、水20質量%以上を少なくとも含むことを特徴とする請求項1及び2に記載の染毛料。
That is, the present invention resides in the following (1) to (3).
(1) At least one kind of acid dye 0.1 to 3% by mass, silica-coated pigment 0.1 to 10% by mass, water resistant resin 0.5 to 3% by mass (solid content), and lower alcohol 20 to 60% by mass, 2 to 20% by mass of hair dyeing aid, 0.5 to 10% by mass of pH adjuster and at least a thickening agent, the viscosity is 40 to 200 mPa·s, and the pH is 2 to 2. A hair dye, which is adjusted to 5.
(2) The silica-coated pigment is obtained by surface-treating at least one selected from black iron oxide, red iron oxide, yellow iron oxide, carbon black, black ink, and titanium oxide with silica. Hair dye as described in.
(3) The hair dye according to claim 1 or 2, wherein the hair dye contains at least 20% by mass of water.
本発明によれば、耐水性に優れると共に、低pH環境下でもシリカ被覆顔料を安定に分散でき、使用直後の洗髪が不要であり、塗布直後の毛髪染毛性に優れるだけでなく、使用する回数を重ねる毎に徐々に毛髪を染色していく累積染毛性、使用性に優れた染毛料が提供される。 According to the present invention, in addition to being excellent in water resistance, the silica-coated pigment can be stably dispersed even in a low pH environment, there is no need to wash hair immediately after use, and not only excellent hair dyeability immediately after application but also use Provided is a hair dye that is excellent in cumulative hair dyeing property and usability, in which hair is gradually dyed as the number of times is repeated.
以下に、本発明の実施の形態を詳しく説明する。
本発明の染毛料は、酸性染料の少なくとも1種0.1〜3質量%と、シリカ被覆顔料0.1〜10質量%と、耐水性樹脂0.5〜3質量%(固形分量)と、低級アルコール20〜60質量%と、染毛助剤2〜20質量%と、pH調整剤0.5〜10質量%と、増粘剤とを少なくとも含み、粘度が40〜200mPa・sであり、pHが2〜5に調整してなることを特徴とするものである。
Hereinafter, embodiments of the present invention will be described in detail.
The hair dye of the present invention comprises at least one kind of acid dye of 0.1 to 3% by mass, a silica-coated pigment of 0.1 to 10% by mass, a water resistant resin of 0.5 to 3% by mass (solid content), Lower alcohol 20 to 60% by mass, hair dyeing aid 2 to 20% by mass, pH adjuster 0.5 to 10% by mass, and a thickener are included at least, and the viscosity is 40 to 200 mPa·s, It is characterized in that the pH is adjusted to 2 to 5.
本発明に用いる酸性染料としては、一般的に化粧品で用いられている法定色素中の酸性染料のうち、少なくとも1種を用いることができる。
酸性染料の具体例としては、赤色2号、赤色3号、赤色102号、赤色104号、赤色105号、赤色106号、黄色4号、黄色5号、緑色3号、青色1号、青色2号、赤色201号、赤色206号、赤色227号、赤色230号、赤色231号、赤色232号、橙色205号、橙色207号、黄色202号、黄色203号、緑色201号、緑色204号、緑色205号、青色202号、青色203号、青色205号、褐色201号、褐色201号、赤色401号、赤色502号、赤色503号、赤色504号、赤色506号、橙色403号、黄色402号、黄色403号の(1)、黄色406号、黄色407号、緑色401号、緑色402号、紫色401号、黒色401号などの少なくとも1種(各単独又は2種以上の混合物、以下、同様)が挙げられる。
これらの酸性染料の含有量は、染毛料全量に対して、0.1〜3質量%(以下、「質量%」を単に「%」という)、好ましくは、0.3〜2%、特に好ましくは、0.3〜1.5%が望ましい。
この酸性染料の含有量が0.1%未満の場合、染毛効果が十分に得られず、一方、3%を超えると、溶解性、保存安定性に悪影響があり、水及び低級アルコールを用いた場合には混合溶媒中への溶解度の影響で、系が不安定になったり、皮膚等への汚染が生じやすくなるため、好ましくない。
As the acidic dye used in the present invention, at least one of the acidic dyes in the legal dyes generally used in cosmetics can be used.
Specific examples of the acid dyes include Red No. 2, Red No. 3, Red No. 102, Red No. 104, Red No. 105, Red No. 106, Yellow No. 4, Yellow No. 5, Green No. 3, Blue No. 1, Blue No. 2 No., Red No. 201, Red No. 206, Red No. 227, Red No. 230, Red No. 231, Red No. 232, Orange No. 205, Orange No. 207, Yellow No. 202, Yellow No. 203, Green No. 201, Green No. 204, Green 205, Blue 202, Blue 203, Blue 205, Brown 201, Brown 201, Red 401, Red 502, Red 503, Red 504, Red 506, Orange 403, Yellow 402 No., yellow No. 403 (1), yellow No. 406, yellow No. 407, green No. 401, green No. 402, purple No. 401, black No. 401, etc., at least one kind (each alone or a mixture of two or more kinds, hereinafter, Same).
The content of these acidic dyes is 0.1 to 3% by mass (hereinafter, "mass%" is simply referred to as "%"), preferably 0.3 to 2%, and particularly preferably, the total amount of the hair dye. Is preferably 0.3 to 1.5%.
When the content of this acid dye is less than 0.1%, the hair dyeing effect is not sufficiently obtained, while when it exceeds 3%, solubility and storage stability are adversely affected, and water and lower alcohols are used. In that case, the system becomes unstable and contamination of the skin and the like is likely to occur due to the influence of the solubility in the mixed solvent, which is not preferable.
本発明に用いるシリカ被覆顔料は、塗布直後の白髪や、希望する着色性などへの一時着色性などを向上させるために用いられるものである。
用いることができるシリカ被覆顔料は、黒酸化鉄、黄色酸化鉄、ベンガラなどの酸化鉄、カーボンブラック、酸化チタン、酸化亜鉛等の無機系の顔料粒子、墨、群青、マイカ、タルクなどの顔料粒子から選ばれる少なくとも1種をシリカで表面処理されたものである。好ましくは、隠ぺい力やコストの面から、黒酸化鉄、黄色酸化鉄、ベンガラなどの酸化鉄やカーボンブラック等の無機顔料粒子から選ばれる少なくとも1種をシリカで表面処理されたものが望ましい。
The silica-coated pigment used in the present invention is used for improving gray hair immediately after coating and temporary coloring property to desired coloring property.
Silica-coated pigments that can be used are black iron oxide, yellow iron oxide, iron oxides such as red iron oxide, carbon black, titanium oxide, inorganic pigment particles such as zinc oxide, black, ultramarine, mica, talc and other pigment particles. At least one selected from the above is surface-treated with silica. From the viewpoint of hiding power and cost, it is preferable that at least one selected from iron oxides such as black iron oxide, yellow iron oxide and red iron oxide, and inorganic pigment particles such as carbon black is surface-treated with silica.
本発明の染毛料においては、酸性染料による染毛性を向上させるため、後述するように、染毛料のpHは2〜5と低く設計している。この影響で用いるシリカ被覆顔料は、時間の経過と共に若干劣化が進み、色調が若干変化してしまうという点が一部に生じる点等から、更に鋭意検討の結果、水と低級アルコール混合溶媒系でも容易にシリカ被覆顔料が分散でき、なおかつpHの影響を更に受けないようにするため、好ましくは、シリカ被覆顔料の平均粒子径が0.3〜3μmとなるものを用いることが望ましい。なお、本発明(後述する実施例)において「平均粒子径」は、シリカ被覆顔料粒子の10重量%分散液を粒径アナライザーFPAR−1000(大塚電子株式会社製)及び粒子径分布測定装置マイクロトラックSIA(マイクロトラック・ベル株式会社製)により測定した値である。 In the hair dye of the present invention, the pH of the hair dye is designed to be as low as 2 to 5, as described later, in order to improve the hair dyeing property with the acid dye. The silica-coated pigment used under this influence is a little deteriorated with the passage of time, and the color tone is slightly changed. Therefore, as a result of further diligent study, even in a mixed solvent system of water and a lower alcohol, In order to easily disperse the silica-coated pigment and not to be further affected by pH, it is preferable to use a silica-coated pigment having an average particle diameter of 0.3 to 3 μm. In the present invention (Examples described later), "average particle size" means a 10 wt% dispersion of silica-coated pigment particles in a particle size analyzer FPAR-1000 (manufactured by Otsuka Electronics Co., Ltd.) and a particle size distribution measuring device Microtrac. It is a value measured by SIA (manufactured by Microtrac Bell Co., Ltd.).
本発明において、上記シリカ被覆顔料の製造は、黒酸化鉄、黄色酸化鉄、ベンガラなどの酸化鉄、カーボンブラック、酸化チタン等の無機系の顔料粒子、墨などの顔料粒子の各表面に、シリカを用いてスプレードライ法や気相蒸着法等により表面処理することでシリカ被覆顔料を得ることができ、また、市販品があれば、それらを使用することもできる。
これらの顔料粒子表面に施すシリカの処理濃度は、処理前後の質量換算で2〜15%、好ましくは、2〜12%であることが望ましい。
このシリカの処理濃度が2%未満の場合は、処理量が不十分で経時による粒子の変質やケーキングが生じてしまうことがあり、一方、処理濃度が15%を超えると、粒子自身が有する色相の効果が低下して一時染毛性が若干低下することがある。
In the present invention, the production of the silica-coated pigment, black iron oxide, yellow iron oxide, iron oxide such as red iron oxide, carbon black, inorganic pigment particles such as titanium oxide, each surface of the pigment particles such as black, silica The silica-coated pigment can be obtained by surface-treating it with a spray-drying method, a vapor-phase vapor deposition method, or the like, and if there is a commercial product, those can be used.
The treatment concentration of silica applied to the surface of these pigment particles is 2 to 15%, preferably 2 to 12% in terms of mass before and after the treatment.
If the treatment concentration of this silica is less than 2%, the treatment amount may be insufficient and the particles may deteriorate or caking over time. On the other hand, if the treatment concentration exceeds 15%, the hue of the particles themselves may be increased. The effect of may decrease and the temporary hair dyeing property may slightly decrease.
本発明におけるシリカ被覆顔料の平均粒子径は、概ね0.3〜3μmであり、好ましくは、0.5〜2μmであることが望ましい。
これらのシリカ被覆顔料の平均粒子径が0.3μm未満の場合は、製造技術上やコストとの面から難しく、特にシリカ被覆顔料の製造は技術的に難しく、コストの問題で用途に適さないものとなり、一方、3μmを超える平均粒子径の場合、櫛による毛髪のコーミングの際に、毛髪に付着したシリカ被覆顔料が容易に剥がれてしまうため、好ましくない。
The average particle diameter of the silica-coated pigment in the present invention is generally 0.3 to 3 μm, preferably 0.5 to 2 μm.
When the average particle diameter of these silica-coated pigments is less than 0.3 μm, it is difficult from the viewpoint of production technology and cost, and particularly, the production of silica-coated pigment is technically difficult, and it is not suitable for use due to cost problems. On the other hand, when the average particle diameter exceeds 3 μm, the silica-coated pigment attached to the hair is easily peeled off when combing the hair with a comb, which is not preferable.
本発明における上記シリカ被覆顔料の含有量は、染毛料全量に対して、0.1〜10%、好ましくは0.5〜5%で、好ましくは、1〜3%であることが望ましい。
これら粒子の含有量が0.1%未満の場合、一時着色性が不十分であり、一方、10%を超えると、シリカの処理濃度と、使用感や風合いが悪化してしまい、好ましくない。
The content of the silica-coated pigment in the present invention is 0.1 to 10%, preferably 0.5 to 5%, and preferably 1 to 3% with respect to the total amount of the hair dye.
If the content of these particles is less than 0.1%, the temporary coloring property is insufficient, while if it exceeds 10%, the treatment concentration of silica and the feeling of use and texture are deteriorated, which is not preferable.
本発明に用いる耐水性樹脂は、形成される被膜が耐水性を有しているものであれば特に限定されず、例えば、(1)下記式(I)で示されるビニル環状アミドのモノマー、下記式(II)で示されるアクリル酸誘導体のモノマー及び下記式(III)で示されるアクリル酸の四級化誘導体のモノマーから重合された三元重合体である樹脂などが挙げられる。 The water-resistant resin used in the present invention is not particularly limited as long as the formed film has water resistance. For example, (1) a vinyl cyclic amide monomer represented by the following formula (I), Examples thereof include a resin that is a terpolymer polymerized from a monomer of an acrylic acid derivative represented by the formula (II) and a monomer of a quaternized derivative of acrylic acid represented by the following formula (III).
好ましくは、水溶性と乾燥後の耐水性の点から、前記樹脂の固形分量の全量を100%とした時に、上記式(I)で示されるビニル環状アミドのモノマーを60〜90%と、上記式(II)で示されるアクリル酸誘導体のモノマーを5〜30%と、上記式(III)で示されるアクリル酸の四級化誘導体のモノマーを1〜30%とから重合された三元重合体からなる樹脂の使用が望ましい。
Preferably, from the viewpoint of water solubility and water resistance after drying, when the total amount of the solid content of the resin is 100%, the vinyl cyclic amide monomer represented by the above formula (I) is 60 to 90%, and A terpolymer polymerized from 5 to 30% of the monomer of the acrylic acid derivative represented by the formula (II) and 1 to 30% of the monomer of the quaternized derivative of the acrylic acid represented by the formula (III). It is preferable to use a resin consisting of
用いることができる三元重合体は、疎水的に改変された陽イオン重合体であり、長鎖アルキルをその中に有する。代表的な三元重合体としては、以下の式を有する。
また、用いる上記式(III)で示されるモノマー(アルキルジメチルアミノプロピルメタクリル酸)は、以下のように上記式(II)で示されるアクリル酸誘導体のモノマー(ジメチルアミノプロピルメタクリル酸、DMAPMA)をトシル化することによって調製することが好ましい。
具体的に用いることができる三元重合体としては、好ましくは、上記式(I)がビニルピロリドン、上記式(II)がジメチルアミノプロピルメタクリルアミド、かつ、上記式(III)がアクリル酸の炭素数12〜18、更に好ましくは炭素数12のアルキル四級化誘導体であり、これらの含有量が式(I)が60〜90%、上記式(II)が5〜30%、かつ上記式(III)が1〜30%とから構成され、その重量平均分子量が200,000〜2,000,000、好ましくは、400,000〜800,000であり、この三元重合体は水溶性であるか、又は水分散性であり、更に、支持体表面上にキャスチングされる場合、明らかな耐湿性の、疎水性フィルムを形成し、そのフィルムは表面活性であり、かつ、加水分解的に安定であり、更に、均質な三元重合体であるものが望ましい。
用いることができる三元重合体の市販品としては、スタイリーゼW−10〔ポリクオタニウム55(ISP社製)を樹脂固型分10%としたもの〕、スタイリーゼW−20〔ポリクオタニウム55(ISP社製)を樹脂固型分20%としたもの〕などが挙げられる。
As a terpolymer that can be specifically used, preferably, the above formula (I) is vinylpyrrolidone, the above formula (II) is dimethylaminopropylmethacrylamide, and the above formula (III) is carbon of acrylic acid. Formula 12 is an alkyl quaternized derivative having 12 to 18 carbon atoms, more preferably 12 carbon atoms, and the content of the formula (I) is 60 to 90%, the formula (II) is 5 to 30%, and the formula (II) is III) is 1 to 30%, its weight average molecular weight is 200,000 to 2,000,000, preferably 400,000 to 800,000, and this terpolymer is water-soluble. Or it is water-dispersible and, when cast on a support surface, forms an apparent moisture-resistant, hydrophobic film which is surface-active and hydrolytically stable. Furthermore, it is desirable that the terpolymer is a homogeneous terpolymer.
Commercially available terpolymers that can be used include Stylize W-10 [Polyquaternium 55 (manufactured by ISP) with resin solid content of 10%], Stylise W-20 [Polyquaternium 55 (manufactured by ISP). In which the resin solid content is 20%] and the like.
これらの耐水性樹脂の含有量は、染毛料全量に対して、固形分量で0.5〜3%、好ましくは、0.5〜2.5%であることが望ましい。
この耐水性樹脂の含有量が0.5%未満の場合は、耐水性が不十分であり、好ましくなく、一方、耐水性樹脂の含有量が3%を超えると、水及び低級アルコールの混合溶媒中へ溶解できなかったり、毛髪塗布後の風合いが悪化するため、好ましくない。
The content of these water resistant resins is 0.5 to 3%, preferably 0.5 to 2.5% in terms of solid content based on the total amount of the hair dye.
When the content of the water resistant resin is less than 0.5%, the water resistance is insufficient, which is not preferable. On the other hand, when the content of the water resistant resin exceeds 3%, a mixed solvent of water and a lower alcohol is used. It is not preferable because it cannot be dissolved in the hair or the texture after applying the hair is deteriorated.
本発明に用いる増粘剤は、塗布性、保存安定性、シリカ被覆顔料の沈降抑制などの点から、後述するように、染毛料の粘度範囲を好適なものとするために用いるものであり、例えば、ヒドロキシエチルセルロース、ヒドロキシプロピルメチルセルロース、ステアロキシヒドロキシプロピルメチルセルロース、ヒドロキシプロピルグアーヒドロキシプロピルトリモニウムクロリド、セルロースにカチオン性官能基を付加したカチオン化セルロースなどのセルロース系増粘剤などが挙げられる。これらの中でも、適正な粘性及び染料の溶解安定性を確保した上で、毛髪に滑らかさ、しなやかさ、しっとり感を付与して感触を改善すると共に、耐水性を向上させるはたらきを有し、しかも、ブラシ体等の塗布体を有する染毛料組成物塗布具に用いた場合には、塗布体に良く絡むので使用性及び塗布性を更に向上させる点から、上記各セルロース系増粘剤の使用が望ましい。 The thickener used in the present invention is used for adjusting the viscosity range of the hair dye, as will be described later, from the viewpoints of applicability, storage stability, and suppression of sedimentation of the silica-coated pigment. Examples thereof include cellulosic thickeners such as hydroxyethyl cellulose, hydroxypropyl methyl cellulose, stearoxy hydroxypropyl methyl cellulose, hydroxypropyl guar hydroxypropyltrimonium chloride, and cationized cellulose obtained by adding a cationic functional group to cellulose. Among these, after ensuring proper viscosity and dissolution stability of the dye, it has a function of imparting smoothness, suppleness, and moisturizing feel to the hair to improve the feel, and also to improve water resistance, and When used in a hair dye composition applicator having an applicator such as a brush, it is entangled well with the applicator, and therefore, the use of each of the above-mentioned cellulosic thickeners is recommended in order to further improve usability and applicability. desirable.
用いることができる増粘剤の市販品としては、ヒドロキシプロピルメチルセルロースでは、NEOVISCO−MC HM4000S(三晶社製)、ステアロキシヒドロキシプロピルメチルセルロースではサンジェロース90L(大同化成工業社製)、ヒドロキシプロピルグアーヒドロキシプロピルトリモニウムクロリドではSANCARE2000(三晶社製社製)、カチオン化セルロースではセルコートSC−230M(ポリクオタニウム10、アクゾノーベル社製)などが挙げられる。 Examples of commercially available thickeners that can be used include NEOVISCO-MC HM4000S (manufactured by Sansei Co., Ltd.) in hydroxypropylmethyl cellulose, and Sangerose 90L (manufactured by Daido Kasei Co., Ltd.) in stearoxyhydroxypropyl methylcellulose, hydroxypropyl guar hydroxy. Examples of propyltrimonium chloride include SANCARE2000 (manufactured by Sansei Co., Ltd.), and examples of cationized cellulose include Cellcoat SC-230M (Polyquaternium 10, manufactured by Akzo Nobel).
本発明における増粘剤の含有量は、後述するように、染毛料の粘度範囲(40〜200mPa・s)に調整して本発明の効果を発揮できる含有量であれば良く、染毛料全量に対して、好適な量で調整される。 The content of the thickener in the present invention may be adjusted so that the effect of the present invention can be exhibited by adjusting the viscosity of the hair dye (40 to 200 mPa·s), as will be described later. On the other hand, it is adjusted by a suitable amount.
本発明の染毛料には、更に、低温安定性、乾燥性、低刺激性などの点から、低級アルコールを含有することが望ましく、また、染毛効果の更なる向上の点から染毛助剤を含有することが望ましい。
本発明に用いる低級アルコールとしては、例えば、エタノール、プロパノール、ブタノール、イソプロパノール、イソブタノール等の揮発性を有する低級アルコールの1種または2種以上を用いることができるが、安全性、乾燥性、匂い等の点からエタノールが望ましい。
これらの低級アルコールの含有量は、染毛料全量に対して、好ましくは、20〜60%、更に好ましくは、20〜55%であり、特に好ましくは30〜50%である。
この低級アルコールの含有量が20%未満の場合、染毛料の乾燥性が低下するため、好ましくなく、一方、60%を超える場合は、累積染毛効果が低下するため、好ましくない。
The hair dye of the present invention preferably further contains a lower alcohol from the viewpoints of stability at low temperature, drying property, and low irritation, and from the viewpoint of further improving the hair dyeing effect, a hair dyeing aid. It is desirable to contain
As the lower alcohol used in the present invention, for example, one or more volatile lower alcohols such as ethanol, propanol, butanol, isopropanol, and isobutanol can be used. Ethanol is desirable from the viewpoint of the above.
The content of these lower alcohols is preferably 20 to 60%, more preferably 20 to 55%, and particularly preferably 30 to 50% based on the total amount of the hair dye.
When the content of this lower alcohol is less than 20%, the drying property of the hair dye is deteriorated, which is not preferable, while when it exceeds 60%, the cumulative hair dyeing effect is deteriorated, which is not preferable.
用いることができる染毛助剤としては、例えば、ベンジルアルコール、フェニルエチルアルコール、フェノシキエタノール、炭酸プロピレン、プロピレングリコール、エトキシジグリコール、N−メチルピロリドン、N−メチル−2ピロリドン等の少なくとも1種が挙げられる。
これらの染毛助剤の含有量は、染毛料全量に対して、好ましくは、2〜20%であり、更に好ましくは、5〜15%が好適である。
この染毛助剤の含有量が2%未満の場合は、更なる染毛効果が不十分であり、一方、20%を超える場合は、染毛料塗布後の乾燥性が低下し、衣服等への色移りの危険性が増すため、好ましくない。
Examples of hair dyeing assistants that can be used include at least one of benzyl alcohol, phenylethyl alcohol, phenoxyethanol, propylene carbonate, propylene glycol, ethoxydiglycol, N-methylpyrrolidone, N-methyl-2pyrrolidone and the like. Are listed.
The content of these hair dyeing aids is preferably 2 to 20%, and more preferably 5 to 15%, based on the total amount of the hair dye.
If the content of this hair dyeing aid is less than 2%, the further hair dyeing effect is insufficient, while if it exceeds 20%, the drying property after application of the hair dyeing agent is reduced, and it is not suitable for clothes. This is not preferable because it increases the risk of color transfer.
本発明における染毛料の残部は、水(精製水、蒸留水、イオン交換水、純水、水道水等)で調整される。
この水の含有量としては、染毛料全量に対して20%以上とすることが必要であり、更に好ましくは、30〜60%である。
この水の含有量が20%未満の場合、染料の溶解性が低下し、染毛効果も低下してしまうため好ましくなく、一方、60%を超えると、含有する耐水性樹脂の安定性が若干低下することがあり、乾燥性が若干低下してしまうことがある。
The balance of the hair dye in the present invention is adjusted with water (purified water, distilled water, ion-exchanged water, pure water, tap water, etc.).
The content of this water needs to be 20% or more, and more preferably 30 to 60%, based on the total amount of the hair dye.
If the content of water is less than 20%, the solubility of the dye is reduced and the hair dyeing effect is also reduced, which is not preferable. On the other hand, if it exceeds 60%, the stability of the water-resistant resin contained is slightly increased. In some cases, the drying property may be slightly deteriorated.
本発明の染毛料の粘度は、適正な粘性及び染料の溶解安定性、毛髪に滑らかさ、しなやかさ、しっとり感を付与して感触を改善すると共に、耐水性の向上、塗布体に用いた場合の使用性及び塗布性を更に向上させる点、ヘアマスカラへの適用の点から、25℃における粘度(ELD粘度計:50rpm)が40〜200mPa・s、好ましくは、50〜150mPa・sとすることが望ましい。
本発明の染毛料において、上記粘度範囲(40〜200mPa・s)の調整は、用いる酸性染料種及びその量、シリカ被覆顔料種及びその量、耐水性樹脂種及びその量、増粘剤種及びその量などを好適に調整することにより調製することができる。
この染毛料の粘度が40mPa・s未満であると、容器等からの液漏れが起きやすくなり、また、頭皮に付着しやすく、また、跳ねて衣服を汚しやすくなり、一方、200mPa・sを越えると、使用者がブラシ等の塗布体に絡まる液量のコントロールをしにくくなり、また、頭髪へ薄く均一に塗り延ばすことがしにくくなり、好ましくない。
The viscosity of the hair dye of the present invention has an appropriate viscosity and dissolution stability of dyes, smoothness, suppleness, and moisturizing the hair to improve the feel, and also to improve the water resistance, when used in a coated body. The viscosity at 25° C. (ELD viscometer: 50 rpm) is from 40 to 200 mPa·s, preferably from 50 to 150 mPa·s, from the viewpoint of further improving the usability and coating properties of the composition and application to hair mascara. Is desirable.
In the hair dye of the present invention, the viscosity range (40 to 200 mPa·s) is adjusted by adjusting the acidic dye species and its amount, the silica-coated pigment species and their amounts, the water-resistant resin species and their amounts, the thickener species and It can be prepared by suitably adjusting the amount and the like.
When the viscosity of this hair dye is less than 40 mPa·s, liquid leaks easily from the container and the like, and it easily adheres to the scalp and splashes to stain clothes, while it exceeds 200 mPa·s. If so, it becomes difficult for the user to control the amount of liquid entangled in the application body such as a brush, and it becomes difficult to apply the liquid thinly and evenly to the hair, which is not preferable.
本発明の染毛料は、着色性向上、皮膚刺激防止、皮膚染着トラブル防止のため、pHを2〜5に調整することが必要であり、好ましくは、pHを2.5〜4.0に調整することが望ましい。
この染毛料のpHが2未満の場合、皮膚染着性が増大するので好ましくなく、一方、pHが5を超える場合は、染毛性が低下し、好ましくない。
本発明において、pHの調整は、蟻酸、酢酸、乳酸、酒石酸、リンゴ酸、クエン酸、グリコール酸等の有機酸や無機酸又はその塩、場合によってはトリエタノールアミンなどのアルカリを用いて行うことができる。これらのpH調整剤はpHが上述の範囲内に収まっていたとしても上記酸性染料の溶存安定性の観点から、その含有量は0.5〜10%、好ましくは、1〜5%である。
The hair dye of the present invention needs to have a pH adjusted to 2 to 5 in order to improve colorability, prevent skin irritation, and prevent skin dyeing trouble, and preferably has a pH of 2.5 to 4.0. It is desirable to adjust.
When the pH of this hair dye is less than 2, it is not preferable because the dyeing property on the skin is increased, and when the pH is more than 5, the hair dyeing property is deteriorated, which is not preferable.
In the present invention, the pH is adjusted by using an organic acid such as formic acid, acetic acid, lactic acid, tartaric acid, malic acid, citric acid or glycolic acid, an inorganic acid or a salt thereof, and in some cases an alkali such as triethanolamine. You can Even if the pH is within the above range, the content of these pH adjusters is 0.5 to 10%, preferably 1 to 5% from the viewpoint of the solubility stability of the acid dye.
本発明の染毛料は、上記酸性染料の少なくとも1種、シリカ被覆顔料、耐水性樹脂、増粘剤、好ましく用いる低級アルコール、染毛助剤、水などの他に、本発明の効果を損なわない範囲で、その他の原材料、例えば、各種界面活性剤、防腐剤、紫外線吸収剤、酸化防止剤、還元防止剤、キレート剤、油性成分、香料、動植物抽出物などを適宜含有することができる。 The hair dye of the present invention does not impair the effects of the present invention in addition to at least one of the above acid dyes, a silica-coated pigment, a water resistant resin, a thickener, a lower alcohol preferably used, a hair dyeing aid, water and the like. Other raw materials such as various surfactants, preservatives, ultraviolet absorbers, antioxidants, anti-reducing agents, chelating agents, oily components, fragrances, animal and plant extracts, etc. can be appropriately contained within the range.
本発明の染毛料は、常法により調製することができ、上記酸性染料の少なくとも1種、シリカ被覆顔料、耐水性樹脂、増粘剤、好ましく用いる低級アルコール、染毛助剤、水などの各成分を上記各含有量の範囲で配合し、更に好適な混練機などを用いて、均一に攪拌・混合することにより、上記粘度範囲、pH範囲となる染毛料が製造することができる。
例えば、耐水性樹脂、低級アルコールなどのアルコール相と、酸性染料と水などの水相とを各々を汎用のディスパーなどにて均一になるまで撹拌後、アルコール相と水相を混合した後、更にpH調整剤、増粘剤などを加え、ディスパーなどにて均一になるまで撹拌後、シリカ被覆顔料を添加し、ホモミキサーなどにて撹拌して、目的の染毛料を調製することができる。
The hair dye of the present invention can be prepared by a conventional method, and includes at least one of the above acid dyes, a silica-coated pigment, a water resistant resin, a thickener, a lower alcohol preferably used, a hair dyeing aid, water and the like. By blending the components in the ranges of the above respective contents and further uniformly stirring and mixing them by using a suitable kneading machine or the like, a hair dye having the above viscosity range and pH range can be produced.
For example, a water-resistant resin, an alcohol phase such as a lower alcohol, and an acidic dye and an aqueous phase such as water are stirred with a general-purpose disper or the like until uniform, and then the alcohol phase and the aqueous phase are mixed, A target hair dye can be prepared by adding a pH adjuster, a thickener and the like, stirring with a disper or the like until uniform, then adding a silica-coated pigment and stirring with a homomixer or the like.
このように構成される本発明の染毛料を使用に供するにあたっては、汎用の毛髪用塗布具を用いることができ、用いる毛髪用塗布具の形状、構造等は特に限定されるものでなく、例えば、ノック式のバルブ装置を備えた塗布具、ヘアマスカラタイプの塗布具、チューブタイプの塗布具、ピストン押圧機構を備えた塗布具などが挙げられる。 A general-purpose hair applicator can be used when using the hair dye of the present invention configured as described above, and the shape, structure, etc. of the hair applicator to be used are not particularly limited. , An applicator having a knock type valve device, a hair mascara type applicator, a tube type applicator, an applicator having a piston pressing mechanism, and the like.
このように構成される本発明の染毛料は、酸性染料の少なくとも1種0.1〜3質量%と、シリカ被覆顔料0.1〜10質量%と、耐水性樹脂0.1〜10質量%と、増粘剤とを少なくとも含み、粘度が40〜200mPa・sであり、pHが2〜5に調整することにより、低pH環境下でもシリカ被覆顔料粒子を安定に分散でき、使用直後の洗髪が不要であり、酸性染料と相まって塗布直後の毛髪染毛性となる一時着色性に優れるだけでなく、使用する回数を重ねる毎に徐々に毛髪を染色していく累積染毛性に優れ、耐水性、使用性、塗布性、低温安定性、乾燥性、低刺激性などに優れた染毛料が得られることとなる。 The hair dye of the present invention thus configured has at least one kind of acid dye of 0.1 to 3% by mass, silica coating pigment of 0.1 to 10% by mass, and water resistant resin of 0.1 to 10% by mass. And a thickener, the viscosity is 40 to 200 mPa·s, and by adjusting the pH to 2 to 5, the silica-coated pigment particles can be stably dispersed even in a low pH environment, and the hair is washed immediately after use. Is not necessary, and it is not only excellent in temporary coloring that becomes hair dyeability immediately after application in combination with acid dye, but also excellent in cumulative hair dyeing that gradually dyes hair as it is used many times, water resistant Therefore, it is possible to obtain a hair dye having excellent properties, usability, coating properties, low temperature stability, drying properties, and low irritation.
次に、実施例により、本発明を更に詳述するが、本発明は下記実施例等により限定されるものではない。 Next, the present invention will be described in more detail with reference to examples, but the present invention is not limited to the following examples.
〔実施例1〜8及び比較例1〜12〕
下記表1に示す配合処方(全量100%)で、汎用のプロペラミキサーなどにより、均一に攪拌・混合して、各染毛料組成物を調製した。
上記で得られた実施例1〜8及び比較例1〜12の各染毛料について、下記方法により、pH、粘度について測定等した。
これらの結果を下記表1に示す。
[Examples 1 to 8 and Comparative Examples 1 to 12]
Each hair dye composition was prepared by uniformly agitating and mixing with a general-purpose propeller mixer or the like according to the formulation (total amount 100%) shown in Table 1 below.
The pH and viscosity of each of the hair dyes obtained in Examples 1 to 8 and Comparative Examples 1 to 12 obtained above were measured by the following methods.
The results are shown in Table 1 below.
(pHの測定方法)
pH(25℃)をガラス電極pH計により常法にて測定した。
(Method of measuring pH)
The pH (25° C.) was measured by a glass electrode pH meter by a conventional method.
(粘度の評価方法)
25℃における各粘度(50rpm)をELD型粘度計、EMD型粘度計、EHD型粘度計(いずれも東機産業社製)にて測定した。なお、12mPa・sを超える粘度はEMD型粘度計にて、256mPa・sを超える粘度はEHD型粘度計にて測定した。
(Viscosity evaluation method)
Each viscosity (50 rpm) at 25° C. was measured with an ELD type viscometer, an EMD type viscometer, and an EHD type viscometer (all manufactured by Toki Sangyo Co., Ltd.). The viscosity exceeding 12 mPa·s was measured with an EMD type viscometer, and the viscosity exceeding 256 mPa·s was measured with an EHD type viscometer.
次いで、上記で得られた各染毛料組成物を用いて、下記方法により、耐水性、一時着色性、累積染毛性(3回)、塗布性、低温安定性、乾燥性、刺激性の評価を行った。また、これらの7評価から下記評価基準で総合評価した。
これらの結果を下記表1に示す。
Then, using each of the hair dye compositions obtained above, evaluation of water resistance, temporary coloring property, cumulative hair dyeing property (3 times), coating property, low temperature stability, drying property, and irritation property by the following methods I went. In addition, comprehensive evaluation was performed based on the following evaluation criteria from these 7 evaluations.
The results are shown in Table 1 below.
(耐水性の評価方法)
2gの山羊毛に約0.4gを塗布し、常温で120分間乾燥後(以下、単に「山羊毛に塗布・乾燥後」という)に、水で湿らせた濾紙を押し当て、濾紙への色の付き具合を、下記評価基準で評価した。
評価基準:
◎:濾紙に全く付着しない。
○:濾紙に若干付着するが問題のない範囲。
△:濾紙にやや濃く付着する。
×:濾紙に濃く付着する。
(Water resistance evaluation method)
Approximately 0.4 g was applied to 2 g of goat hair, dried at room temperature for 120 minutes (hereinafter simply referred to as "after applied and dried on goat hair"), and then pressed with a filter paper moistened with water to color the filter paper. Was evaluated according to the following evaluation criteria.
Evaluation criteria:
⊚: Does not adhere to the filter paper at all.
◯: A range in which there is no problem although it slightly adheres to the filter paper.
Δ: Attached to the filter paper in a slightly thicker color.
X: Thickly adheres to the filter paper.
(一時着色性の評価方法)
1gの人毛白髪に約0.2gを塗布し、常温で120分間乾燥後(以下、単に「人毛白髪に塗布・乾燥後」という)に、目視で観察し、下記評価基準で評価した。
を、下記評価基準で評価した。
評価基準:
◎:自然な白髪ではない毛髪と遜色が無い。
○:上記◎より若干薄い。
△:着色しているがやや薄い。
×:はっきりと薄い。
(Temporary colorability evaluation method)
About 0.2 g was applied to 1 g of human white hair, dried at room temperature for 120 minutes (hereinafter, simply referred to as “after applied to human hair and dried”), visually observed, and evaluated according to the following evaluation criteria.
Was evaluated according to the following evaluation criteria.
Evaluation criteria:
⊚: Same as hair that is not natural gray.
◯: Slightly thinner than ◎ above.
Δ: Colored but slightly light.
X: Clearly thin.
(累積染毛性の評価方法)
1gの毛髪毛束に塗布・乾燥後、二回洗髪を3回繰り返し後の、累積染毛性の評価を下記評価基準で評価した。
評価基準:
◎:市販の酸化染毛料と同等。
○:市販の酸化染毛料に若干劣る。
△:やや染まりにくい。
×:染まらない。
(Evaluation method for cumulative hair dyeability)
After applying to 1 g of a hair bundle and drying, and then washing twice with hair three times, the cumulative dyeability was evaluated according to the following evaluation criteria.
Evaluation criteria:
A: Equivalent to commercially available oxidative hair dye.
◯: Slightly inferior to commercially available oxidative hair dye.
Δ: Difficult to dye.
X: Does not stain.
(塗布性の評価方法)
マスカラタイプの塗布具、具体的には、有底筒状体となる塗布具本体(PP製)の上端開口部を螺合により密封する蓋体とを備え、その内部に本発明の染毛料の貯蔵槽(ボトルタイプ)となる貯留部を有すると共に、該貯留部の上部には払拭部が取り付けられ、しかも、蓋体は塗布棒が固着され、該塗布棒の先端にはブラシ体が所定間隔毎に多数有する塗布体(SUS−304製の軸、ナイロン製のブラシ)を有する塗布具により、毛髪に塗布した際の塗布性を下記評価基準で評価した。
評価基準:
◎:毛髪へ付着する液量が良好であり、良好な塗布性を有していた。
○:毛髪へ付着する液量が良好であり、塗布性が上記◎より若干劣る。
△:毛髪へ付着する液量がやや減り、若干塗布性が上記○より劣る。
×:毛髪へ付着する液量が減り、塗布性が悪い。
(Evaluation method of coating property)
A mascara type applicator, specifically, a lid body for sealing an upper end opening of an applicator body (made of PP) which is a bottomed tubular body by screwing, and inside of the hair dye of the present invention. In addition to having a storage part that serves as a storage tank (bottle type), a wiping part is attached to the upper part of the storage part, and a coating rod is fixed to the lid body, and a brush body is attached to the tip of the coating rod at predetermined intervals. The applicability when applied to the hair was evaluated by the following evaluation criteria with an applicator having a large number of applicators (a shaft made of SUS-304, a brush made of nylon).
Evaluation criteria:
⊚: The amount of liquid adhering to the hair was good, and the coatability was good.
◯: The amount of liquid adhering to the hair is good, and the coatability is slightly inferior to ◎ above.
Δ: The amount of liquid adhering to the hair is slightly reduced, and the coatability is slightly inferior to the above ○.
X: The amount of liquid adhering to the hair is reduced and the coatability is poor.
(低温安定性の評価方法)
各染毛料100mlを蓋付き透明容器に入れ、−10℃、1ヶ月で保存後、肉眼で下記評価基準で評価した。
評価基準:
◎:沈殿物がなく、製造後と同様の状態を維持している。
○:沈殿物は若干あるが、上記◎より若干劣るが許容の範囲。
△:沈殿物がややあるが、品質、使用性に問題がないレベル。
×:沈降(沈殿物)がある。
(Evaluation method of low temperature stability)
100 ml of each hair dye was placed in a transparent container with a lid, stored at −10° C. for 1 month, and evaluated visually with the following evaluation criteria.
Evaluation criteria:
⊚: There is no precipitate and the same state as after production is maintained.
◯: Some precipitates, but slightly inferior to ◎ above, but within the allowable range.
Δ: There is a slight amount of precipitate, but there is no problem in quality and usability.
X: There is sedimentation (precipitate).
(塗布後の乾燥性の評価方法)
25℃−65RH%下で、1gの人毛白髪の毛束に0.2gを塗布し、30秒毎に指で触れ、指への付着がなくなる時間を測定し、下記評価基準で評価した。
評価基準:
◎:2分以内
○:2.5分以内
△:4分以内
×:4分超過
(Evaluation method of dryness after coating)
0.2 g was applied to a hair bundle of 1 g of human white hair at 25° C.-65 RH%, and touched with a finger every 30 seconds, the time at which the finger was no longer attached was measured, and evaluated according to the following evaluation criteria.
Evaluation criteria:
◎: Within 2 minutes ○: Within 2.5 minutes △: Within 4 minutes ×: Over 4 minutes
(刺激性の評価方法)
実施例1〜8、比較例1〜12のうち、比較例3〜4を除く塗布可能な18サンプルについて、モニター20人の皮膚の出来るだけ近い位置で、塗布を行い、刺激を感じるかどうかの確認を行い、下記評価基準で評価した。
評価基準:
◎:刺激を感じたモニターは0人だった。
○:1人のモニターが刺激を感じた。
△:2〜6人のモニターが刺激を感じた。
×:7人以上のモニターが刺激を感じた。
(Stimulation method)
Of Examples 1 to 8 and Comparative Examples 1 to 12, 18 samples that can be applied except Comparative Examples 3 and 4 were applied at positions as close as possible to the skin of 20 monitors, and whether irritation was felt It confirmed and evaluated by the following evaluation criteria.
Evaluation criteria:
⊚: There were no monitors who felt irritation.
○: One monitor felt irritation.
Δ: Monitors of 2 to 6 people felt irritation.
×: 7 or more monitors felt irritation.
(総合評価方法)
上記耐水性、一時着色性、累積染毛性(3回)、塗布性、低温安定性、乾燥性及び刺激性の各評価(7評価)から下記評価基準で評価した。
評価基準:
◎:塗布性能が◎評価で、他の各評価もすべて◎評価のもの。
○:塗布性能が◎評価で、他の各評価も△評価がなく、○評価以上のもの。
△:塗布性能が◎評価又は○評価であっても、他の評価に△評価1以上のもの、または、塗布性能以外の各評価が○以上の評価であっても、塗布性能が△評価の場合。
×:×評価が1個以上のもの、または、評価できなかったもの。
(Comprehensive evaluation method)
The following evaluation criteria were evaluated from the respective evaluations (7 evaluations) of the water resistance, temporary coloring property, cumulative hair dyeing property (3 times), coating property, low temperature stability, drying property and irritation property.
Evaluation criteria:
⊚: The coating performance is ◎, and all other evaluations are ◎.
◯: The coating performance was evaluated as ⊚, the other evaluations were not evaluated as Δ, and the evaluation was ◯ or higher.
Δ: The coating performance was evaluated as ⊚ or ○, and the other evaluations were evaluated as 1 or more, or the coating performance was evaluated as Δ even if each evaluation other than the coating performance was evaluated as ○ or more. If.
×: × One or more evaluations, or one that could not be evaluated.
上記表1中の*1〜*8は、下記のとおりである。
*1:12%−シリカ処理黒酸化鉄、平均粒子径2μm(日揮触媒化成株式会社製)
*2:12%−シリカ処理べんがら、平均粒子径0.5μm(日揮触媒化成株式会社製)
*3:10%−シリカ処理黄酸化鉄、平均粒子径0.5μm(日揮触媒化成株式会社製)
*4:ヒドロキシプロピルメチルセルロース(三晶社製社製)
*5:ステアロキシヒドロキシプロピルメチルセルロース(大同化成工業社製)
*6:ヒドロキシプロピルグアーヒドロキシプロピルトリモニウムクロリド(三晶社製)
*7:カチオン化セルロース(アクゾノーベル社製)
*8:スタイリーゼW−10〔ポリクオタニウム55(ISP社製、樹脂固形分10%)〕
*1 to *8 in Table 1 above are as follows.
*1: 12%-silica-treated black iron oxide, average particle size 2 μm (manufactured by JGC Catalysts & Chemicals Co., Ltd.)
*2: 12%-silica-treated red iron oxide, average particle size 0.5 μm (manufactured by JGC Catalysts & Chemicals Co., Ltd.)
*3: 10%-silica-treated yellow iron oxide, average particle diameter 0.5 μm (manufactured by JGC Catalysts & Chemicals Co., Ltd.)
*4: Hydroxypropyl methylcellulose (manufactured by Sansho Co., Ltd.)
*5: Stearoxyhydroxypropyl methylcellulose (manufactured by Daido Kasei Co., Ltd.)
*6: Hydroxypropyl guar Hydroxypropyltrimonium chloride (manufactured by Sansei Co.)
*7: Cationized cellulose (manufactured by Akzo Nobel)
*8: Stylize W-10 [Polyquaternium 55 (manufactured by ISP, resin solid content 10%)]
上記表1の結果から明らかなように、本発明範囲となる実施例1〜8は、本発明の範囲外となる比較例1〜12に較べ、耐水性、一時着色性、累積染毛性(3回)、塗布性、低温安定性、乾燥性、低刺激性に優れ、これらが高度に両立した染毛料となることが判明した。
また、実施例1〜8の各染毛料は、塗布直後の染毛性、累積染毛性の評価結果などから、低pH環境下でも、一時着色時の色相と累積染毛時の色相とのズレがなく、白髪などへの一時着色性能、累積染毛性能に優れることが判った。
これに対して、比較例を個別的に見ると、比較例1はシリカ被覆顔料を含有しない場合であり、比較例2は染毛量の粘度が低い場合であり、比較例3及び4は低級アルコール(エタノール)の量が本発明の範囲外となる場合であり、比較例5及び6は酸性染料の量が本発明の範囲外となる場合であり、比較例7及び8はpH調整剤の量が本発明の範囲外となる場合であり、比較例9及び10は染毛助剤の量が本発明の範囲外となる場合であり、比較例11及び12は耐水性樹脂の量が本発明の範囲外となる場合であり、これらの場合は、本発明の効果を発揮できないことが判った。また、比較例3,4は、沈降し、上記の各評価はできなかった。
As is clear from the results in Table 1 above, Examples 1 to 8, which fall within the scope of the present invention, have water resistance, temporary colorability, and cumulative hair dyeing property (compared with Comparative Examples 1 to 12 that fall outside the scope of the present invention). 3 times), it was found that the coatability, low temperature stability, drying property, and low irritation are excellent, and that these are highly compatible hair dyes.
In addition, from the evaluation results of the hair dyeing properties immediately after application, the cumulative hair dyeing properties, etc., the hair dyes of Examples 1 to 8 show that the hue during temporary coloring and the hue during cumulative hair dyeing are low even in a low pH environment. It was found that there was no deviation, and the ability to temporarily color gray hair and the like and cumulative hair dyeing performance were excellent.
On the other hand, when looking at Comparative Examples individually, Comparative Example 1 is a case where the silica-coated pigment is not contained, Comparative Example 2 is a case where the viscosity of the hair dye amount is low, and Comparative Examples 3 and 4 are low. When the amount of alcohol (ethanol) is outside the range of the present invention, Comparative Examples 5 and 6 are cases where the amount of acid dye is outside the range of the present invention, and Comparative Examples 7 and 8 are those of the pH adjusting agent. When the amount is outside the range of the present invention, Comparative Examples 9 and 10 are cases where the amount of hair dyeing aid is outside the range of the present invention, and Comparative Examples 11 and 12 are when the amount of water resistant resin is the same. This is a case outside the scope of the invention, and it was found that the effects of the present invention cannot be exhibited in these cases. Further, in Comparative Examples 3 and 4, sedimentation occurred, and the above evaluations could not be performed.
耐水性に優れると共に、低pH環境下でもシリカ被覆顔料を安定に分散でき、使用直後の洗髪が不要であり、塗布直後の毛髪染毛性に優れるだけでなく、使用する回数を重ねる毎に徐々に毛髪を染色していく累積染毛性、使用性に優れる染毛料となるので、ノック式のバルブ装置を備えた塗布具、ヘアマスカラタイプの塗布具、チューブタイプの塗布具、ピストン押圧機構を備えた塗布具に収容して好適に用いることができる。 In addition to being excellent in water resistance, the silica-coated pigment can be stably dispersed even in a low pH environment, there is no need to wash hair immediately after use, and it not only excels in hair dyeability immediately after application, but also gradually with each use. As it is a hair dye with excellent cumulative hair dyeing property and usability, it is possible to use an applicator equipped with a knock type valve device, a hair mascara type applicator, a tube type applicator, and a piston pressing mechanism. It can be suitably used by accommodating it in a provided applicator.
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