CA2347861C - Wrinkle reduction laundry product compositions - Google Patents
Wrinkle reduction laundry product compositions Download PDFInfo
- Publication number
- CA2347861C CA2347861C CA002347861A CA2347861A CA2347861C CA 2347861 C CA2347861 C CA 2347861C CA 002347861 A CA002347861 A CA 002347861A CA 2347861 A CA2347861 A CA 2347861A CA 2347861 C CA2347861 C CA 2347861C
- Authority
- CA
- Canada
- Prior art keywords
- formulation
- sodium
- detergent
- wrinkle
- sulphated
- 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
Links
- 239000000203 mixture Substances 0.000 title claims description 80
- 230000037331 wrinkle reduction Effects 0.000 title description 16
- 239000003599 detergent Substances 0.000 claims abstract description 41
- 230000037303 wrinkles Effects 0.000 claims abstract description 39
- 238000009472 formulation Methods 0.000 claims description 54
- 239000003638 chemical reducing agent Substances 0.000 claims description 15
- 239000004094 surface-active agent Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 9
- 239000008158 vegetable oil Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000004359 castor oil Substances 0.000 claims description 7
- 235000019438 castor oil Nutrition 0.000 claims description 7
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 7
- 235000019519 canola oil Nutrition 0.000 claims description 3
- 239000000828 canola oil Substances 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 abstract description 21
- 230000008901 benefit Effects 0.000 abstract description 8
- 238000004140 cleaning Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 239000004744 fabric Substances 0.000 description 29
- 150000001875 compounds Chemical class 0.000 description 26
- -1 alkyl amides Chemical class 0.000 description 23
- 239000007844 bleaching agent Substances 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 108091005804 Peptidases Proteins 0.000 description 13
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 102000004190 Enzymes Human genes 0.000 description 11
- 108090000790 Enzymes Proteins 0.000 description 11
- 229940088598 enzyme Drugs 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 10
- 230000003750 conditioning effect Effects 0.000 description 10
- 239000010457 zeolite Substances 0.000 description 10
- 239000002243 precursor Substances 0.000 description 9
- 239000004365 Protease Substances 0.000 description 8
- 229910021536 Zeolite Inorganic materials 0.000 description 8
- 125000000217 alkyl group Chemical group 0.000 description 8
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
- 229910052708 sodium Inorganic materials 0.000 description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 7
- 229910000503 Na-aluminosilicate Inorganic materials 0.000 description 7
- 102000035195 Peptidases Human genes 0.000 description 7
- 239000002304 perfume Substances 0.000 description 7
- 239000000344 soap Substances 0.000 description 7
- 235000012217 sodium aluminium silicate Nutrition 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 239000004115 Sodium Silicate Substances 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 150000004996 alkyl benzenes Chemical class 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 6
- 229910052911 sodium silicate Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000004753 textile Substances 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 5
- 102000004882 Lipase Human genes 0.000 description 5
- 108090001060 Lipase Proteins 0.000 description 5
- 229910052783 alkali metal Inorganic materials 0.000 description 5
- 125000003342 alkenyl group Chemical group 0.000 description 5
- 229910000323 aluminium silicate Inorganic materials 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 5
- 239000000835 fiber Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000002736 nonionic surfactant Substances 0.000 description 5
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 5
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229920013822 aminosilicone Polymers 0.000 description 4
- 230000001153 anti-wrinkle effect Effects 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 4
- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 239000006081 fluorescent whitening agent Substances 0.000 description 4
- 239000000314 lubricant Substances 0.000 description 4
- 150000004965 peroxy acids Chemical class 0.000 description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 4
- 229920000058 polyacrylate Polymers 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 239000000429 sodium aluminium silicate Substances 0.000 description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 4
- 229940045872 sodium percarbonate Drugs 0.000 description 4
- 239000000600 sorbitol Substances 0.000 description 4
- 239000003381 stabilizer Substances 0.000 description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 4
- 239000004367 Lipase Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 3
- 239000003945 anionic surfactant Substances 0.000 description 3
- 238000004061 bleaching Methods 0.000 description 3
- UZABCLFSICXBCM-UHFFFAOYSA-N ethoxy hydrogen sulfate Chemical compound CCOOS(O)(=O)=O UZABCLFSICXBCM-UHFFFAOYSA-N 0.000 description 3
- 235000019421 lipase Nutrition 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229940024999 proteolytic enzymes for treatment of wounds and ulcers Drugs 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 239000003826 tablet Substances 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 108010059892 Cellulase Proteins 0.000 description 2
- 244000060011 Cocos nucifera Species 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 108010056079 Subtilisins Proteins 0.000 description 2
- 102000005158 Subtilisins Human genes 0.000 description 2
- 229920006243 acrylic copolymer Polymers 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- 150000001860 citric acid derivatives Chemical class 0.000 description 2
- STNGULMWFPMOCE-UHFFFAOYSA-N ethyl 4-butyl-3,5-dimethyl-1h-pyrrole-2-carboxylate Chemical compound CCCCC1=C(C)NC(C(=O)OCC)=C1C STNGULMWFPMOCE-UHFFFAOYSA-N 0.000 description 2
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000010409 ironing Methods 0.000 description 2
- 238000004900 laundering Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 2
- 229920005646 polycarboxylate Polymers 0.000 description 2
- 229920005996 polystyrene-poly(ethylene-butylene)-polystyrene Polymers 0.000 description 2
- 239000011253 protective coating Substances 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 125000001453 quaternary ammonium group Chemical group 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- 229960000999 sodium citrate dihydrate Drugs 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- 239000002888 zwitterionic surfactant Substances 0.000 description 2
- CFPOJWPDQWJEMO-UHFFFAOYSA-N 2-(1,2-dicarboxyethoxy)butanedioic acid Chemical class OC(=O)CC(C(O)=O)OC(C(O)=O)CC(O)=O CFPOJWPDQWJEMO-UHFFFAOYSA-N 0.000 description 1
- BDKLKNJTMLIAFE-UHFFFAOYSA-N 2-(3-fluorophenyl)-1,3-oxazole-4-carbaldehyde Chemical compound FC1=CC=CC(C=2OC=C(C=O)N=2)=C1 BDKLKNJTMLIAFE-UHFFFAOYSA-N 0.000 description 1
- GIVLOEWMYMRPJA-UHFFFAOYSA-N 2-[carboxymethyl(ethyl)amino]-2-hydroxyacetic acid Chemical class OC(=O)CN(CC)C(O)C(O)=O GIVLOEWMYMRPJA-UHFFFAOYSA-N 0.000 description 1
- JBNHKYQZNSPSOR-UHFFFAOYSA-N 4-(carboxymethylperoxy)-4-oxobutanoic acid Chemical class OC(=O)CCC(=O)OOCC(O)=O JBNHKYQZNSPSOR-UHFFFAOYSA-N 0.000 description 1
- XSVSPKKXQGNHMD-UHFFFAOYSA-N 5-bromo-3-methyl-1,2-thiazole Chemical compound CC=1C=C(Br)SN=1 XSVSPKKXQGNHMD-UHFFFAOYSA-N 0.000 description 1
- 102000013142 Amylases Human genes 0.000 description 1
- 108010065511 Amylases Proteins 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 241000194108 Bacillus licheniformis Species 0.000 description 1
- 235000014469 Bacillus subtilis Nutrition 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical group [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 102000005701 Calcium-Binding Proteins Human genes 0.000 description 1
- 108010045403 Calcium-Binding Proteins Proteins 0.000 description 1
- 108010084185 Cellulases Proteins 0.000 description 1
- 102000005575 Cellulases Human genes 0.000 description 1
- RKWGIWYCVPQPMF-UHFFFAOYSA-N Chloropropamide Chemical compound CCCNC(=O)NS(=O)(=O)C1=CC=C(Cl)C=C1 RKWGIWYCVPQPMF-UHFFFAOYSA-N 0.000 description 1
- OCUCCJIRFHNWBP-IYEMJOQQSA-L Copper gluconate Chemical class [Cu+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O OCUCCJIRFHNWBP-IYEMJOQQSA-L 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- SCKXCAADGDQQCS-UHFFFAOYSA-N Performic acid Chemical compound OOC=O SCKXCAADGDQQCS-UHFFFAOYSA-N 0.000 description 1
- 108700020962 Peroxidase Proteins 0.000 description 1
- 102000003992 Peroxidases Human genes 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical class OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- BGRWYDHXPHLNKA-UHFFFAOYSA-N Tetraacetylethylenediamine Chemical compound CC(=O)N(C(C)=O)CCN(C(C)=O)C(C)=O BGRWYDHXPHLNKA-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 235000019418 amylase Nutrition 0.000 description 1
- 229940025131 amylases Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
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- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229910052816 inorganic phosphate Inorganic materials 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000002366 lipolytic effect Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 108010003855 mesentericopeptidase Proteins 0.000 description 1
- 108010020132 microbial serine proteinases Proteins 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N n-hexanoic acid Natural products CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 150000004967 organic peroxy acids Chemical class 0.000 description 1
- 125000005342 perphosphate group Chemical group 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003138 primary alcohols Chemical class 0.000 description 1
- 230000002797 proteolythic effect Effects 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 229940087562 sodium acetate trihydrate Drugs 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 description 1
- 229960001922 sodium perborate Drugs 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- QUCDWLYKDRVKMI-UHFFFAOYSA-M sodium;3,4-dimethylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1C QUCDWLYKDRVKMI-UHFFFAOYSA-M 0.000 description 1
- IBDSNZLUHYKHQP-UHFFFAOYSA-N sodium;3-oxidodioxaborirane;tetrahydrate Chemical compound O.O.O.O.[Na+].[O-]B1OO1 IBDSNZLUHYKHQP-UHFFFAOYSA-N 0.000 description 1
- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 150000003890 succinate salts Chemical class 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
- C11D3/3738—Alkoxylated silicones
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/83—Mixtures of non-ionic with anionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/34—Organic compounds containing sulfur
- C11D3/3472—Organic compounds containing sulfur additionally containing -COOH groups or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
- C11D3/3742—Nitrogen containing silicones
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3769—(Co)polymerised monomers containing nitrogen, e.g. carbonamides, nitriles or amines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/29—Sulfates of polyoxyalkylene ethers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
Abstract
The present application relates to the inclusion of one or more wrinkle reducing ingredients in a laundry detergent product. The benefits are delivered to the laundered item during the cleaning step and, therefore, reduces the need for further wrinkle reducing steps when the items are taken from the dryer or after hang drying.
Description
C6514 (C) WO
Amended 23 January 2001 LAIINDRY PRODUCT COMPOSITIONS
Technical Field The present invention relates to laundry product compositions for reducing fabric wrinkling.
Background of the Invention When textiles, such as clothing, linens and the like, are laundered, it is typically desired that wrinkles be eliminated or minimized after the cleaning and drying process. Mechanical wrinkle reduction techniques, such as heat and pressure (for example, ironing), have been used but can be time consuming and inconvenient.
Known attempts to reduce wrinkles by means of chemical ingredients in the wash include the use of zwitterionic surfactants, aminosilicones, curable aminosilicones, cellulase enzymes and alkyl amides. However, each of these ingredients have one or more drawbacks. For example, zwitterionic surfactants are believed to work best in cold water. Aminosilicones can cause yellowing and can be difficult to formulate. Curable aminosilicones require the heat of an iron to reduce wrinkles. Cellulase enzymes generally require several wash cycles before anti-wrinkle benefits become noticeable. Alkyl amides are not very effective relative to other wrinkle reducing agents.
Therefore, there is a need for an effective and efficient means for eliminating or reducing wrinkles in textiles. To AMENDED SHEET
C6514 (C) WO
Amended 23 January 2001 be effective and efficient, the ingredient should preferably work across a-broad range of water temperatures, not require the use of an iron, have little to no discoloration effect on the laundered item and/or provide a noticeable wrinkle reducing benefit after relatively few wash cycles.
US-A-3992332 discloses a liquid composition for treatment and reconditioning of fabrics, including from 1 to 10% by weight of a water soluble silicone glycol copolymer of nonionic series group consisting of polyoxyethylene polymethylsiloxane and polyoxyethylene polyoxypropylene polymethylsiloxane, from 5 to 20% by weight of a fibre coupling antistatic phosphate derivative of anionic series from 0.5 to 5% by weight of a detergent and from 55 to 93.4%
by weight of water.
WO-A-94/07980 discloses an aqueous fabric cleaning shampoo composition containing from 0.05% to 5% by weight of a silicone betaine polymer.
US-A-4846982 relates to a particulate fabric laundering detergent formulation comprising a mixture of a fabric softening conditioning compound consisting of a polydimethylsiloxane polymer and polyoxyalkylene siloxane copolymer.
US-A-5645751 relates to a fabric finish concentrate composition comprising water, a water soluble polymer and a silicone ironing aid/lubricant., AM E%2~~ IS rEET=
- 2a -GB-A-2200365 describes a detergent composition comprising a detersive active mixture consisting of a combination of conventional. surfactants and one or more mutually compatible silicone containing compounds of nonionic or amphoteric nature.
US-A-3918983 relates to a composotion comprising a sulphated mixture of alcohol and unsaturated oils (e.g.'vegetable oils) excluding castor oil.
XP-002128906 pertains to a textile softener composition containing 10 to 20% by weight of a sodium salt Qf sulphated castor oil.
Statement of Invention The present application relates to the inclusion of one or more wrinkle reducing ingredients in a laundry detergent product.
Thus, a first aspect of the present invention provides a powdered or table detergent formulation comprising a wrinkle reducing agent selected from one or more of sulphated vegetable oils and sulphonated vegetable oils;
said laundry detergent formulation comprising from 15 to 60 wt% of surfactant.
-2b-The benefits are delivered to the laundered item during cleaning; this reduces the need for further wrinkle reducing steps when the items are taken from the dryer or after hang drying.
Amended 23 January 2001 LAIINDRY PRODUCT COMPOSITIONS
Technical Field The present invention relates to laundry product compositions for reducing fabric wrinkling.
Background of the Invention When textiles, such as clothing, linens and the like, are laundered, it is typically desired that wrinkles be eliminated or minimized after the cleaning and drying process. Mechanical wrinkle reduction techniques, such as heat and pressure (for example, ironing), have been used but can be time consuming and inconvenient.
Known attempts to reduce wrinkles by means of chemical ingredients in the wash include the use of zwitterionic surfactants, aminosilicones, curable aminosilicones, cellulase enzymes and alkyl amides. However, each of these ingredients have one or more drawbacks. For example, zwitterionic surfactants are believed to work best in cold water. Aminosilicones can cause yellowing and can be difficult to formulate. Curable aminosilicones require the heat of an iron to reduce wrinkles. Cellulase enzymes generally require several wash cycles before anti-wrinkle benefits become noticeable. Alkyl amides are not very effective relative to other wrinkle reducing agents.
Therefore, there is a need for an effective and efficient means for eliminating or reducing wrinkles in textiles. To AMENDED SHEET
C6514 (C) WO
Amended 23 January 2001 be effective and efficient, the ingredient should preferably work across a-broad range of water temperatures, not require the use of an iron, have little to no discoloration effect on the laundered item and/or provide a noticeable wrinkle reducing benefit after relatively few wash cycles.
US-A-3992332 discloses a liquid composition for treatment and reconditioning of fabrics, including from 1 to 10% by weight of a water soluble silicone glycol copolymer of nonionic series group consisting of polyoxyethylene polymethylsiloxane and polyoxyethylene polyoxypropylene polymethylsiloxane, from 5 to 20% by weight of a fibre coupling antistatic phosphate derivative of anionic series from 0.5 to 5% by weight of a detergent and from 55 to 93.4%
by weight of water.
WO-A-94/07980 discloses an aqueous fabric cleaning shampoo composition containing from 0.05% to 5% by weight of a silicone betaine polymer.
US-A-4846982 relates to a particulate fabric laundering detergent formulation comprising a mixture of a fabric softening conditioning compound consisting of a polydimethylsiloxane polymer and polyoxyalkylene siloxane copolymer.
US-A-5645751 relates to a fabric finish concentrate composition comprising water, a water soluble polymer and a silicone ironing aid/lubricant., AM E%2~~ IS rEET=
- 2a -GB-A-2200365 describes a detergent composition comprising a detersive active mixture consisting of a combination of conventional. surfactants and one or more mutually compatible silicone containing compounds of nonionic or amphoteric nature.
US-A-3918983 relates to a composotion comprising a sulphated mixture of alcohol and unsaturated oils (e.g.'vegetable oils) excluding castor oil.
XP-002128906 pertains to a textile softener composition containing 10 to 20% by weight of a sodium salt Qf sulphated castor oil.
Statement of Invention The present application relates to the inclusion of one or more wrinkle reducing ingredients in a laundry detergent product.
Thus, a first aspect of the present invention provides a powdered or table detergent formulation comprising a wrinkle reducing agent selected from one or more of sulphated vegetable oils and sulphonated vegetable oils;
said laundry detergent formulation comprising from 15 to 60 wt% of surfactant.
-2b-The benefits are delivered to the laundered item during cleaning; this reduces the need for further wrinkle reducing steps when the items are taken from the dryer or after hang drying.
A further aspect of the present invention provides a method of reducing the occurrence of wrinkles in laundered clothing comprising:
providing a detergent formulation according to the first aspect of the invention;
contacting the detergent formulation with clothing during a washing procedure;
and allowing the clothing'to dry.
The laundered clothing has fewer wrinkles present than the same clothing if laundered and dried in the same or similar manner with a*detergent formulation which is identical, except that it does not include'the wrinkle-reducing agent.
The'product can be provided in any suitable form, for example, as a powder, liquid or tablet. Delivery can be achieved by direct dosing,..drawer dispensing or by other known dosing means. Tablets can also be dosed in mesh bags.
The ingredients that facilitate the benefit of wrinkle reduction are believed to lubricate fiber surfaces. By 'lubricating the fiber surfaces of garments, for=example, the fibers slide more easily relative to each other and are less likely to entangle, resulting in less wrinkles. The preferred fiber lubricants disclosed herein have been shown to noticeably reduce the number of wrinkles. The preferred embodiments also overcome one or more of the above noted disadvantages of prior wrinkle reducing agents or methods.
While it is known that lubricants can be used to reduce wrinkles in textiles, it was surprisingly found that these materials work from a main wash detergent. More particularly, main wash detergents are highly diluted and are subject to one or more rinse cycles. Such high dilution and rinsing would be expected to diminish or eliminate the desired wrinkle reduction effect of the lubricant.
Detailed Description of the Invention Several molecules have been identified for wrinkle reduction benefits when included in known liquid detergent formulations. Using the American Association of Textile Chemists and Colorists (AATCC) method# 124 (described in greater detail, below), the claimed molecular classes were found to reduce the number of wrinkles on test cloths. A
preferred wrinkle reducing agent is a polyalkyleneoxide modified polydimethylsiloxane, for example that sold under the name Silwet" L-7622, available from Witco, Greenwich, CT.
Other most preferred wrinkle reducing agents are sulphated canola oil and/or castor oil available from Freedom Chemical Co., Charlotte, NC.
One or more of the molecules/compounds from the above-identified classes are preferably included in known detergent formulations in an effective amount sufficing to reduce the occurrence of wrinkles as compared to clothing laundered and dried in a similar manner with a detergent formulation that excludes the wrinkle reducing agents. An effective amount of the wrinkle reducing ingredient is preferably from 0.l.wt% to 10 wtt, more preferably from 0.1 wt% to 5 wt% and most preferably from 0.3 wt% to I.S.
wtt. Suitable liquid detergent formulations are described;
= = .
for example,'in U.S. Patent Nos.: 4,261,868; 4,322,308;
4,959,179; 5,089,163; 5,147,576; and 5,205,957.
An additional advantage of the above-identified wrinkle reducing ingredients is that the molecules/compounds do not have a net positive charge in a neutral or alkaline medium, i.e. a medium having a pH greater than or equal to about 6.5. Lack of a net=positive charge makes their inclusion in liquid detergents containing anionic surfactants much easier. More specifically, they are less likely to precipitate=with negatively charged surfactants. =
A further,advantage is the likelihood of "yellowing"*fabrics with the above wrinkle reducing molecules is less than with amine-containinig, ingredients. In addition, some of the above wrinkle reducing ingredients, such as sulphated vegetable oils, are relatively inexpensive.
The detergent formulations of the invention may contain a , .
surface-active compound (surfactant)'which may be chosen from=soap and non-soap anionic, cationic, non-ionic, amphoteric and zwitterionic surface-active compounds and mixtures thereof. Many suitable surface-active compounds are available and are fully described in the=literature, for C6514 (C) WO
Amended 23 January 2001 example, in "Surface-Active Agents and Detergents", Volumes I and II, by Schwartz, Perry and Berch.
The preferred detergent-active compounds that can be used are soaps and synthetic non-soap anionic and non-ionic compounds.
The formulations of the invention may contain linear alkylbenzene sulphonate, particularly linear alkylbenzene sulphonates having an alkyl chain length of C8-C15. It is preferred if the level of linear alkylbenzene sulphonate 'is from 0 wt% to 30 wt%, more preferably 1 wt% to 25 wt%, most preferably from 2 wt% to 15 wt%.
The formulations of the invent'ion may contain other anionic surfactants in amounts additional to the percentages quoted above. Suitable anionic surfactants are well-known to those skilled in the art. Examples include primary and secondary alkyl sulphates, particularly C8-C15 primary alkyl sulphates;
alkyl ether sulphates; olefin sulphonates; alkyl xylene sulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates. Sodium salts are generally preferred.
The formulations of the invention may also contain non-ionic surfactant. Nonionic surfactants that may be used include the primary and secondary alcohol ethoxylates, especially the C8-C20 aliphatic alcohols ethoxylated with an average of from 1 to 20 moles of ethylene oxide per mole of alcohol, and more especially the C1o-C15 primary and secondary A,Lrc,;D
SHFET
C6514 (C) WO
Amended 23 January 2001 aliphatic alcohols ethoxylated with an average of from 1 to moles of ethylene oxide per mole of alcohol. Non-ethoxylated nonionic surfactants include alkylpoly-glycosides, glycerol monoethers, and polyhydroxyamides 5 (glucamide).
It is preferred if the level of non-ionic surfactant is from 0 wt% to 30 wt%, preferably from 1 wt% to 25 wt%, most' preferably from 2 wt% to 15 wt%.
The choice of surface-active compound (surfactant), and the amount present, will depend on the intended use of the detergent composition. In fabric washing compositions, different surfactant systems may be chosen, as is well known to the skilled formulator, for handwashing products and for products intended for use in different types of washing machine.
The total amount of surfactant present will also depend on the intended end use and may be as high as 60 wt%, for example, in a composition for washing fabrics by hand. In compositions for machine washing of fabrics, an amount of from 5 to 40 wt% is generally appropriate. Typically the compositions will comprise at least 2 wt% surfactant e.g. 2-60%,'preferably 15-40% most preferably 5-35%.
Detergent formulations suitable for use in most automatic fabric washing machines generally contain anionic, non-soap surfactant, or non-ionic surfactant, or combinations of the two in any suitable ratio, optionally together with soap.
L;.
A":;r,u`
,J St1EET
C6514 (C) WO
Amended 23 January 2001 Conventional fabric conditioning compound may optionally be used in the formulations of the present invention. The conditioning compounds may be cationic or non-ionic. If the fabric conditioning compound is to be employed in a main wash detergent composition the compound will typically be non-ionic. For rinse cycle products, it will typically be cationic. The term fabric conditioning compound as used herein includes fabric softening compounds or.agents.
The fabric conditioning compound is suitably a substantially water insoluble quaternary ammonium material comprising a single alkyl or alkenyl long chain having an average chain length greater than or equal to C20 or, more preferably, a compound comprising a polar head group and two alkyl or alkenyl chains having an average chain length greater than or equal to C14.
Preferably the fabric conditioning compound has two long chain alkyl or alkenyl chains each having an average chain length greater than or equal to C16. Most preferably at least 50% of the long chain alkyl or alkenyl groups have a chain length of C18 or above. It is preferred if the long chain alkyl or alkenyl groups of the fabric conditioning compounds are predominantly linear.
The fabric conditioning compounds which optionally may be used in the formulations of the invention are preferably compounds that provide excellent softening and are characterised by a chain melting Lp to La transition F%,,~t:Dg) SNEET
C6514 (C) WO
Amended 23 January 2001 temperature greater than 25 C, preferably greater than 35 C, most preferably greater than 45 C.= This'L(3 to La transition can be,measured by DSC as defined in "Handbook of Lipid .,Bilayers,. D Marsh, CRC Press, Boca Raton, Florida, 1990 (pages 137 and 337).
Substantially insoluble fabric conditioning-compounds in the context of this invention are defined as fabric conditioning compounds having a solubility less than 1 x 10-3 wt% in demineralised water at 20 C. Preferably the fabric softening compounds have a solubility less than 1 x 10 4 wt%, most preferably less than 1 x 10-8 to 1 x 106.
The formulations of the invention, when used as main wash fabric washing compositions, will generally also contain one or more detergency builders. The total amount of detergency builder in the compositions will typically range from 5 to 80 wt%, preferably from 10 to 60 wt%.
Inorganic builders that may be present include sodium carbonate, if desired in combination with a crystallisation seed for calcium carbonate, as disclosed in GB 1 437 950' (Unilever); crystalline and amorphous aluminosilicates, for example, zeolites as disclosed in GB 1 473 201 (Henkel), amorphous aluminosilicates as disclosed in GB.1 473 202 (Henkel) and mixed crystalline/amorphous aluminosilicates as disclosed in GB 1 470 250 (Procter & Gamble); and layered silicates as disclosed in EP 164 514B (Hoechst). Inorganic phosphate builders, for example, sodium orthophosphate, SNEET
~t:DLD
C6514 (C) WO
Amended 23 January 2001 -pyrophosphate and tripolyphosphate are also suitable for use with this invention.
The formulations of the invention preferably contain an 5 alkali metal, preferably sodium aluminosilicate builder.
Sodium aluminosilicates may generally be incorporated in amounts of from 10 to 70% by weight (anhydrous basis), preferably from 25 to 50 wt%.
providing a detergent formulation according to the first aspect of the invention;
contacting the detergent formulation with clothing during a washing procedure;
and allowing the clothing'to dry.
The laundered clothing has fewer wrinkles present than the same clothing if laundered and dried in the same or similar manner with a*detergent formulation which is identical, except that it does not include'the wrinkle-reducing agent.
The'product can be provided in any suitable form, for example, as a powder, liquid or tablet. Delivery can be achieved by direct dosing,..drawer dispensing or by other known dosing means. Tablets can also be dosed in mesh bags.
The ingredients that facilitate the benefit of wrinkle reduction are believed to lubricate fiber surfaces. By 'lubricating the fiber surfaces of garments, for=example, the fibers slide more easily relative to each other and are less likely to entangle, resulting in less wrinkles. The preferred fiber lubricants disclosed herein have been shown to noticeably reduce the number of wrinkles. The preferred embodiments also overcome one or more of the above noted disadvantages of prior wrinkle reducing agents or methods.
While it is known that lubricants can be used to reduce wrinkles in textiles, it was surprisingly found that these materials work from a main wash detergent. More particularly, main wash detergents are highly diluted and are subject to one or more rinse cycles. Such high dilution and rinsing would be expected to diminish or eliminate the desired wrinkle reduction effect of the lubricant.
Detailed Description of the Invention Several molecules have been identified for wrinkle reduction benefits when included in known liquid detergent formulations. Using the American Association of Textile Chemists and Colorists (AATCC) method# 124 (described in greater detail, below), the claimed molecular classes were found to reduce the number of wrinkles on test cloths. A
preferred wrinkle reducing agent is a polyalkyleneoxide modified polydimethylsiloxane, for example that sold under the name Silwet" L-7622, available from Witco, Greenwich, CT.
Other most preferred wrinkle reducing agents are sulphated canola oil and/or castor oil available from Freedom Chemical Co., Charlotte, NC.
One or more of the molecules/compounds from the above-identified classes are preferably included in known detergent formulations in an effective amount sufficing to reduce the occurrence of wrinkles as compared to clothing laundered and dried in a similar manner with a detergent formulation that excludes the wrinkle reducing agents. An effective amount of the wrinkle reducing ingredient is preferably from 0.l.wt% to 10 wtt, more preferably from 0.1 wt% to 5 wt% and most preferably from 0.3 wt% to I.S.
wtt. Suitable liquid detergent formulations are described;
= = .
for example,'in U.S. Patent Nos.: 4,261,868; 4,322,308;
4,959,179; 5,089,163; 5,147,576; and 5,205,957.
An additional advantage of the above-identified wrinkle reducing ingredients is that the molecules/compounds do not have a net positive charge in a neutral or alkaline medium, i.e. a medium having a pH greater than or equal to about 6.5. Lack of a net=positive charge makes their inclusion in liquid detergents containing anionic surfactants much easier. More specifically, they are less likely to precipitate=with negatively charged surfactants. =
A further,advantage is the likelihood of "yellowing"*fabrics with the above wrinkle reducing molecules is less than with amine-containinig, ingredients. In addition, some of the above wrinkle reducing ingredients, such as sulphated vegetable oils, are relatively inexpensive.
The detergent formulations of the invention may contain a , .
surface-active compound (surfactant)'which may be chosen from=soap and non-soap anionic, cationic, non-ionic, amphoteric and zwitterionic surface-active compounds and mixtures thereof. Many suitable surface-active compounds are available and are fully described in the=literature, for C6514 (C) WO
Amended 23 January 2001 example, in "Surface-Active Agents and Detergents", Volumes I and II, by Schwartz, Perry and Berch.
The preferred detergent-active compounds that can be used are soaps and synthetic non-soap anionic and non-ionic compounds.
The formulations of the invention may contain linear alkylbenzene sulphonate, particularly linear alkylbenzene sulphonates having an alkyl chain length of C8-C15. It is preferred if the level of linear alkylbenzene sulphonate 'is from 0 wt% to 30 wt%, more preferably 1 wt% to 25 wt%, most preferably from 2 wt% to 15 wt%.
The formulations of the invent'ion may contain other anionic surfactants in amounts additional to the percentages quoted above. Suitable anionic surfactants are well-known to those skilled in the art. Examples include primary and secondary alkyl sulphates, particularly C8-C15 primary alkyl sulphates;
alkyl ether sulphates; olefin sulphonates; alkyl xylene sulphonates; dialkyl sulphosuccinates; and fatty acid ester sulphonates. Sodium salts are generally preferred.
The formulations of the invention may also contain non-ionic surfactant. Nonionic surfactants that may be used include the primary and secondary alcohol ethoxylates, especially the C8-C20 aliphatic alcohols ethoxylated with an average of from 1 to 20 moles of ethylene oxide per mole of alcohol, and more especially the C1o-C15 primary and secondary A,Lrc,;D
SHFET
C6514 (C) WO
Amended 23 January 2001 aliphatic alcohols ethoxylated with an average of from 1 to moles of ethylene oxide per mole of alcohol. Non-ethoxylated nonionic surfactants include alkylpoly-glycosides, glycerol monoethers, and polyhydroxyamides 5 (glucamide).
It is preferred if the level of non-ionic surfactant is from 0 wt% to 30 wt%, preferably from 1 wt% to 25 wt%, most' preferably from 2 wt% to 15 wt%.
The choice of surface-active compound (surfactant), and the amount present, will depend on the intended use of the detergent composition. In fabric washing compositions, different surfactant systems may be chosen, as is well known to the skilled formulator, for handwashing products and for products intended for use in different types of washing machine.
The total amount of surfactant present will also depend on the intended end use and may be as high as 60 wt%, for example, in a composition for washing fabrics by hand. In compositions for machine washing of fabrics, an amount of from 5 to 40 wt% is generally appropriate. Typically the compositions will comprise at least 2 wt% surfactant e.g. 2-60%,'preferably 15-40% most preferably 5-35%.
Detergent formulations suitable for use in most automatic fabric washing machines generally contain anionic, non-soap surfactant, or non-ionic surfactant, or combinations of the two in any suitable ratio, optionally together with soap.
L;.
A":;r,u`
,J St1EET
C6514 (C) WO
Amended 23 January 2001 Conventional fabric conditioning compound may optionally be used in the formulations of the present invention. The conditioning compounds may be cationic or non-ionic. If the fabric conditioning compound is to be employed in a main wash detergent composition the compound will typically be non-ionic. For rinse cycle products, it will typically be cationic. The term fabric conditioning compound as used herein includes fabric softening compounds or.agents.
The fabric conditioning compound is suitably a substantially water insoluble quaternary ammonium material comprising a single alkyl or alkenyl long chain having an average chain length greater than or equal to C20 or, more preferably, a compound comprising a polar head group and two alkyl or alkenyl chains having an average chain length greater than or equal to C14.
Preferably the fabric conditioning compound has two long chain alkyl or alkenyl chains each having an average chain length greater than or equal to C16. Most preferably at least 50% of the long chain alkyl or alkenyl groups have a chain length of C18 or above. It is preferred if the long chain alkyl or alkenyl groups of the fabric conditioning compounds are predominantly linear.
The fabric conditioning compounds which optionally may be used in the formulations of the invention are preferably compounds that provide excellent softening and are characterised by a chain melting Lp to La transition F%,,~t:Dg) SNEET
C6514 (C) WO
Amended 23 January 2001 temperature greater than 25 C, preferably greater than 35 C, most preferably greater than 45 C.= This'L(3 to La transition can be,measured by DSC as defined in "Handbook of Lipid .,Bilayers,. D Marsh, CRC Press, Boca Raton, Florida, 1990 (pages 137 and 337).
Substantially insoluble fabric conditioning-compounds in the context of this invention are defined as fabric conditioning compounds having a solubility less than 1 x 10-3 wt% in demineralised water at 20 C. Preferably the fabric softening compounds have a solubility less than 1 x 10 4 wt%, most preferably less than 1 x 10-8 to 1 x 106.
The formulations of the invention, when used as main wash fabric washing compositions, will generally also contain one or more detergency builders. The total amount of detergency builder in the compositions will typically range from 5 to 80 wt%, preferably from 10 to 60 wt%.
Inorganic builders that may be present include sodium carbonate, if desired in combination with a crystallisation seed for calcium carbonate, as disclosed in GB 1 437 950' (Unilever); crystalline and amorphous aluminosilicates, for example, zeolites as disclosed in GB 1 473 201 (Henkel), amorphous aluminosilicates as disclosed in GB.1 473 202 (Henkel) and mixed crystalline/amorphous aluminosilicates as disclosed in GB 1 470 250 (Procter & Gamble); and layered silicates as disclosed in EP 164 514B (Hoechst). Inorganic phosphate builders, for example, sodium orthophosphate, SNEET
~t:DLD
C6514 (C) WO
Amended 23 January 2001 -pyrophosphate and tripolyphosphate are also suitable for use with this invention.
The formulations of the invention preferably contain an 5 alkali metal, preferably sodium aluminosilicate builder.
Sodium aluminosilicates may generally be incorporated in amounts of from 10 to 70% by weight (anhydrous basis), preferably from 25 to 50 wt%.
10 The alkali metal aluminosilicate may be either crystalline or amorphous or mixtures thereof, having the general formula: 0.8-1.5 Na20. A1203. 0.8-6 SiO2, These materials contain some bound water and are required to have a calcium ion exchange capacity of at least 50 mg CaO/g. The preferred sodium aluminosilicates contain 1.5-3.5 SiO2 units (in the formula above). Both the amorphous and the crystalline materials can be prepared readily by reaction between sodium silicate and sodium aluminate, as amply described in the literature. Suitable crystalline sodium aluminosilicate ion-exchange detergency builders are described, for example, in GB 1 429 143 (Procter & Gamble).
The preferred sodium aluminosilicates of this type are the well-known commercially available zeolites A and X, and mixtures thereof.
The zeolite may be the commercially available zeolite 4A now widely used in laundry detergent powders. However, according to a preferred embodiment of the invention, the zeolite builder incorporated in the compositions of the SHEET
C6514 (C) WO
Amended 23 January 2001 " - 11 -invention is maximum aluminium zeolite P (zeolite MAP) as described and claimed in EP 384 070A (Unilever). Zeolite MAP is defined as an alkali metal aluminosilicate of the .zeolite P type having.a silicon to aluminium ratio not exceeding 1.33, preferably within the range of from 0.90 to 1.33, and more preferably within the range of from 0.90 to 1.20.
Especially preferred is zeolite MAP having a silicon to aluminium ratio not exceeding 1.07, more preferably about 1.00. The calcium binding capacity of zeolite MAP is generally at least 150 mg CaO per g of anhydrous material.
Organic builders that may be present include polycarboxylate polymers such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphinates; monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono=, di and trisuccinates, carboxymethyloxy succinates, carboxymethloxymalonates, dipicolinates, hydroxy-ethyliminodiacetates, alkyl- and alkenlymalonates and succinates; and sulphonated fatty acid salts. This list is not intended to be exhaustive.
Especially preferred organic builders are citrates, suitably used in amounts of from 5 to 30 wt%, preferably from 10 to 25 wt%; and acrylic polymers, more especially acrylic/maleic copolymers, suitably used in amounts of from 0.5 to 15 wt%, preferably from 1 to 10 wt%.
Builders, both inorganic and organic, are preferably present in alkali metal salt, especially sodium salt, form.
AMENDED SHEET
C6514 (C) WO
Amended 23 January 2001 Formulations according to the invention may also 'suitably contain a bleach system. Fabric washing compositions may desirably contain peroxy bleach compounds; for example, inorganic persalts or organic peroxyacids, capable of yielding hydrogen peroxide in aqueous solution.
Suitable peroxy bleach compounds include organic peroxides such as urea peroxide, and inorganic persalts such as-the alkali metal perborates, percarbonates, perphosphates, persilicates and persulphates. Preferred inorganic persalts are sodium perborate monohydrate and tetrahydrate, and sodium percarbonate.
Especially preferred is sodium percarbonate having a protective coating against destabilisation by moisture.
Sodium percarbonate having a protective coating comprising sodium metaborate and sodium silicate is disclosed in GB 2 123 044B (Kao).
The peroxy bleach compound is suitably present in an amount of from 0.1 to 35 wt%, preferably from 0.5 to 25 wt%. The peroxy bleach compound may be used in conjunction with a bleach activator (bleach precursor) to improve bleaching action at low wash temperatures. The bleach precursor is suitably present in an amount of from 0.1 to 8 wt%, preferably from 0.5 to 5 wt%.
Preferred bleach precursors are peroxycarboxylic acid precursors, more especially peracetic acid precursors and pernoanoic acid precursors. Especially preferred bleach DED SHEE~
C6514 (C) WO
Amended 23 January 2001 precursors suitable for use in the present invention are N,N,N',N.-tetracetyl ethylenediamine (TAED) and sodium noanoyloxybenzene sulphonate (SNOBS). The novel quaternary ammonium and phosphonium bleach precursors disclosed in US 4 751 015 and US 4 818 426 (Lever Brothers Company) and EP 402 971A (Unilever), and the cationic bleach precursors disclosed in EP 284 292A and EP 303 520A (Kao) are also of interest.
The bleach system can be either supplemented with or replaced by a peroxyacid. Examples of such peracids can be found in US 4 686 063 and US 5 397 501 (Unilever). A
preferred example is the imido peroxycarboxylic class of peracids described in EP A 325 288, EP A 349 940, DE 382 3172 and EP 325 289. A particularly preferred example is phtalimido peroxy caproic acid (PAP). Such peracids are suitably present at 0.1 - 12%, preferably 0.5 -10%.
A bleach stabiliser (heavy metal sequestrant) may also be present. Suitable bleach stabilisers include ethylenediamine tetra-acetate (EDTA), the polyphosphonates such as Dequest (Trade Mark) and non-phosphate stabilisers such as EDDS (ethylene diamine di-succinic acid). These bleach stabilisers are also useful for stain removal especially in products containing low levels of bleaching species or no bleaching species.
An especially preferred bleach system comprises a peroxy bleach compound (preferably sodium percarbonate optionally ANENDED SHEET
C6514 (C) WO
Amended 23 January 2001 together with a bleach activator), and a transition metal bleach catalyst as described and claimed in EP 458 397A,.
EP 458 398A and EP 50-9 787A (Unilever).
Formulations according to the invention may also contain one or more enzyme(s). Suitable enzymes include the proteases, amylases, cellulases, oxidases, peroxidases and lipases usable for incorporation in detergent compositions.
Preferred proteolytic enzymes (proteases) are, catalytically active protein materials which degrade or alter protein types of stains when pre,sent as in fabric stains in a hydrolysis reaction. They may be of any suitable origin, such as vegetable, animal, bacterial or yeast origin.
Proteolytic enzymes or proteases of various qualities and origins and'having activity in various pH ranges of from.4-12 are available and can be used in the instant invention.
Examples of suitable proteolytic enzymes are the stabilisins which are obtained from particular strains of B. Subtilis B.
licheniformis, such as the commercially available subtilisins Maxatase (Trade Mark), as supplied by Gist Brocades N.V., Delft, Holland, and Alcalase (Trade Mark), as supplied by Novo Industri A/S, Copenhagen, Denmark.
Particularly suitable is a protease obtained from a strain of Bacillus having maximum activity throughout the pH range of 8-12, being commercially available, e.g. from Novo Industri A/S under the registered trade-names Esperase =(Trade Mark) and Savinase (Trade-Mark). The preparation of these and analogous enzymes is described in GB 1 243 785.
Other commercial proteases are Kazusase (Trade Mark AMENDED SNEET
C6514 (C) WO
Amended 23 January 2001 obtainable from Showa-Denko of Japan), Optimase (Trade Mark from Miles Kali-Chemie, Hannover, West Germany), and Superase (Trade Mark obtainable from Pfizer of U.S.A.).
Detergency enzymes are commonly employed in granular form in amounts of from about 0.1 to about 3.0 wt%. However, any suitable physical form of enzyme may be used.
Other materials that may be present in detergent formulations of the invention include sodium silicate;
antiredeposition agents such as cellulosic polymers;
inorganic salts such as sodium sulphate; lather control agents or lather boosters as appropriate; proteolytic and lipolytic enzymes; dyes; coloured speckles; perfumes; foam controllers; fluorescers and decoupling polymers. This list is not intended to be exhaustive.
It is often advantageous if soil release polymers are present.
Test Method and Examples Wrinkle reduction was measured by using the American Association of Textile Chemists and Colorists' (AATCC) method #124, Appearance of Fabrics after Repeated Home Laundering. In this method, four cloth types (silk, rayon, cotton, and linen) are washed, dried and stored in a well defined way. The dried cloths are then evaluated for wrinkle content by comparison with wrinkle smoothness replicas which can be purchases from AATCC. Factors such as the light used, the angle of the cloths and replicas to the h;~~ENME D SNEE?
- 16 - ' light, and the background are carefully controlled and described in the method. There are six replicas with values of 1, 2, 3, 3.5, 4, and 5 with 5 being=perfectly smooth and 1 being very wrinkled. Three trained observers a're asked to give a value.of 1-5, to the nearest 0.5 unit, to each cloth based on which replica it most closely resembles. The results are totalled and averaged over the three observers for each cloth type. According to the'method, a difference of greater than 0.17 between the results for two products indicates there is a significant difference at the 95%
confidence level. A difference of greater than or equal to 0.25 indicates a significant difference at the 99%
confidence level.
FXample 1 The following formulation containing a wrinkle reduction ingredient was produced: = -Formulation 1 ingredient Percent in Formula (by weight) Sodium alcohol ethoxy aulphate 11.0 9E0 alcohol ethoxylate 6.0 Sodium linear alkyl benzene sulphonate 6.0 Propylene glycol 4.0 Sorbitol 3.5 Borax" 2.0 Sodium citrate 1.5 =
Silwet L-7622* 1.0 -Protease enzyme 0.25 Lipase enzyme 0.5 Water to 100$
* Wrinkle reduction agent - polyoxyalkylene modified C6514 (C) WO
Amended 23 January 2001 polydimethylsiloxane from Witco Chemical.Co.
Formulation 2(the same as formulation 1 without the wrinkle reduction agent present) was also produced.
One wash with each detergerit was performed using 111.4g of detergent in 17 gallons (77.27 litres) of water at 95F
(35 C). In each wash, cotton swatches were included along =
with six pounds (2.72 kg)of cotton ballast. The cotton swatches were used to determine the level of wrinkle reduction.
Wrinkle reduction results gave a wrinkle score of 1.78 for the L-7622-containing detergent and 1.17 for the control.
These results indicate a statistical win for the detergent containing L-7622 at the 99% confidence level.
Example 2 The following formulation containing a wrinkle reduction ingredient was produced:
AM~f <~~~ SHEET
Formulation 3 Ingredient Percent in Formula Sodium alcohol ethoxy sulphate 11.0 9EO alcohol ethoxylate 6.0 Sodium linear alkyl benzene'sulphonate 6.0 Propylene glycol 4.0 Sorbitol 3.5 Borax 2.0 Sodium citrate 1.5 Freedom Scan-75- 1.0 Protease enzyme 0.25 Lipase enzyme 0.5 Water To 100$
*Wrinkle reduction agent - sulphated canola oil from Freedom Chemical Co.
Fozmulation 4 (the same as formulation 3 without the wrinkle reduction agent present) was also produced.
One wash with each detergent was performed using 111.4g of detergent in 17 gallons (77.27 litres) of water at 95F
(35 C). In each wash, silk swatches were included along with six pounds (2.72 kg) of cotton ballast. The silk swatches were used to determine the level of wrinkle reduction.
Wrinkle reduction results gave a wrinkle score of 2.89 for =15 the Freedom Scano 75-containing detergent and 2.39 for the control.
These results indicate a statistical win for the detergent containing Freedom'Scano-75 at the 99lr confidence level.
C6514 (C) WO
Amended 23 January 2001 The following formulations show preferred ranges of ingredients in accordance with the present disclosure.
Formluations.5 and 7 represent detergents having ethoxylated organosilicone copolymers as the wrinkle reducing agent while formulations 6 and 8 represent detergents having sulphated castor oil as the wrinkle reducing agent., Formulations 9 and 10 represent powdered and tabulated formulations, respectfully.
AMENDED SHEET
C6514 (C) WO
Amended 23 January 2001 Formulation 5 Ingredient - Chemical Name Percent in Formula (Based on 100W
Active Raw) Alcohol Ethoxylate 4.0 - 15.0 Sodium alkyl ethoxy sulphate . 7.0 - 25.0 Alkylbenzene sulphonic acid 4.0 - 15.0 Sodium Hydroxide 0.3 - 2.5 Propylene glycol 2.0 - 10.0 Sorbitol 2.0 - 10.0 Sodium Tetraborate Pentahydrate 2.0 - 10.0 Sodium Citrate Dihydrate 1.5 - 10.0 Ethoxylated Organosilicone 0.5 - 5,.0 Copolymer Coconut Fatty Acid 0.4 - 2.5 Fluorescent Whitening Agent 0.1 - 0.6 Antiredeposition Agent 0.15 - 1.5 Enzyme - Protease 0.15 - 1.5 Enzyme - Lipase 0 - 2.0 Monoethanolamine 0.1 - 1.5 Perfume 0.1 - 1.0 Water to 100%
AMENDED SHEET
C6514. (C) WO
Amended 23 January 2001 Formulation 6 Ingredient - Chemical Name Percent in Formula (Based on 100t Active Raw) Alcohol Ethoxylate 4.0 - 15.0 Sodium Alkyl Ethoxy Sulphate 7.0 - 25.0 Alkylbenzene Sulphonic Acid 4.0 - 15.0 Sodium Hydroxide 0.3 - 2.5 Propylene Glycol 2.0 - 10.0 Sorbitol 2.0 - 10.0 Sodium Tetraborate Pentahydrate 2.0 - 10.0 Sodium Citrate Dihydrate 1.5 - 10.0 Sulphated=Castor Oil 0.5 - 10.0 Coconut Fatty Acid 0.4 - 2.5 Fluorescent Whitening Agent 0.1 - 0.6 Antiredeposition Agent 0.15 - 1.5 Enzyme - Protease 0.15 - 1.5 Enzyme - Lipase 0 - 2.0 Monoethanolamine 0.1 - 1.5 Perfume 0.1 - 1.0 Water to 100%
AN~D 4 D4p SriEET
C6514 (C) WO
Amended 23 January 2001 Formulation 7 Ingredient - Chemical Name Percent in Formula (Based on 100%
Active Raw) Alcohol Ethoxylate 3.5 - 20.0 Alkylbenzene Sulphonic Acid 9.5 - 30.0 Sodium Hydroxide 1.0 - 10.0 Ethoxylated Organosilicone 0.5 - 5.0 Copolymer Sodium Xylene Siulphonate 0.75 - 10.0 Stearic Acid 0.09 - 0.5 Sodium Silicate 2.0 - 12.0 Fluorescent Whitening Agent 0.04 - 0.4 Perfume 0.1 - 1.0 Water to 100~
Formulation 8 Ingredient - Chemical Name Percent in Formula (Based on 100%
Active Raw) Alcohol Ethoxylate 3.5 - 20.0 Alkylbenzene Sulphonic Acid 9.5 - 30.0 Sodium Hydroxide 1.0 - 10.0 Sulphated Castor Oil 0.5 - 10.0 Sodium Xylene Sulphonate 0.75 - 10.0 Stearic Acid 0.09 - 0.5 Sodium Silicate 2.0 - 12.0 Fluorescent Whitening Agent 0.04 - 0.4 Perfume 0.1 - 1.0 Water to 100t AMENIDED SHEET
C6514 (C) WO
Amended 23 January 2001 Formulation 9 (Detergent Powder) Linear alkylbenzene sulphonate 13.8%
(LAS) Ethoxylated nonionics (5 to 15 5.2%
moles EO) Sodium aluminosilicate 28%
Sodium carbonate 20%
Sodium sulphate 1896 Sodium silicate 0.5%
Polyacrylates 1.4 Sodium perborate 0 to 8%
Protease enzyme 0.5%
Perfume 0.4%
Fluorescent Whitener 0.3%
Anti-Wrinkle agent See Table A
Water and miscellaneous To 100%
AMENDED SNE.F1 C6514 (C) WO
Amended 23 January 2001 Formulation 10 (Detergent Tablet) Linear alkylbenzene sulphonate 9.4%
Ethoxylated nonionics (5 to 15 mole 4%
EO) Sodium aluminosilicate 254k Sodium carbonate 24.5$
Sodium sulphate 5.4%
Sodium Acetate trihydrate 2596 Fluorescent Whitener 0.316 Stearic soap 0.75%
Perfume 0.4%
Protease enzyme 0.5%
Polyacrylates 1.2%
Anti-wrinkle ingredients See Table A
Water and miscellaneous To 100%
Table A (Anti-wrinkle Ingredients) Ethoxylated organosilicones 1-10%
Polyalkyleneoxide modified 1-10%
polydimethylsiloxane Linear aminopolydimethylsiloxane 1-10%
polyalkyeneoxides Sulphated oil 1-10%
Components in Table A can either be used individually or in combination with the total level being preferably between 1 to 10%.
While the above-identified wrinkle reducing agents are preferably incorporated in detergent compositions, they can also be used in other formulations, such as in rinse treatments or other garment care products.
A,~AEt+D~D SHEET
C6514 (C) WO
Amended 23 January 2001 All component percentages are based on weight, unless otherwise indicated. All numerical values are considered to be modified by the term "about" and should be given the broadest available range of equivalents when construing the claims.
AiA~P1~;~ D S~~~C?
The preferred sodium aluminosilicates of this type are the well-known commercially available zeolites A and X, and mixtures thereof.
The zeolite may be the commercially available zeolite 4A now widely used in laundry detergent powders. However, according to a preferred embodiment of the invention, the zeolite builder incorporated in the compositions of the SHEET
C6514 (C) WO
Amended 23 January 2001 " - 11 -invention is maximum aluminium zeolite P (zeolite MAP) as described and claimed in EP 384 070A (Unilever). Zeolite MAP is defined as an alkali metal aluminosilicate of the .zeolite P type having.a silicon to aluminium ratio not exceeding 1.33, preferably within the range of from 0.90 to 1.33, and more preferably within the range of from 0.90 to 1.20.
Especially preferred is zeolite MAP having a silicon to aluminium ratio not exceeding 1.07, more preferably about 1.00. The calcium binding capacity of zeolite MAP is generally at least 150 mg CaO per g of anhydrous material.
Organic builders that may be present include polycarboxylate polymers such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphinates; monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono=, di and trisuccinates, carboxymethyloxy succinates, carboxymethloxymalonates, dipicolinates, hydroxy-ethyliminodiacetates, alkyl- and alkenlymalonates and succinates; and sulphonated fatty acid salts. This list is not intended to be exhaustive.
Especially preferred organic builders are citrates, suitably used in amounts of from 5 to 30 wt%, preferably from 10 to 25 wt%; and acrylic polymers, more especially acrylic/maleic copolymers, suitably used in amounts of from 0.5 to 15 wt%, preferably from 1 to 10 wt%.
Builders, both inorganic and organic, are preferably present in alkali metal salt, especially sodium salt, form.
AMENDED SHEET
C6514 (C) WO
Amended 23 January 2001 Formulations according to the invention may also 'suitably contain a bleach system. Fabric washing compositions may desirably contain peroxy bleach compounds; for example, inorganic persalts or organic peroxyacids, capable of yielding hydrogen peroxide in aqueous solution.
Suitable peroxy bleach compounds include organic peroxides such as urea peroxide, and inorganic persalts such as-the alkali metal perborates, percarbonates, perphosphates, persilicates and persulphates. Preferred inorganic persalts are sodium perborate monohydrate and tetrahydrate, and sodium percarbonate.
Especially preferred is sodium percarbonate having a protective coating against destabilisation by moisture.
Sodium percarbonate having a protective coating comprising sodium metaborate and sodium silicate is disclosed in GB 2 123 044B (Kao).
The peroxy bleach compound is suitably present in an amount of from 0.1 to 35 wt%, preferably from 0.5 to 25 wt%. The peroxy bleach compound may be used in conjunction with a bleach activator (bleach precursor) to improve bleaching action at low wash temperatures. The bleach precursor is suitably present in an amount of from 0.1 to 8 wt%, preferably from 0.5 to 5 wt%.
Preferred bleach precursors are peroxycarboxylic acid precursors, more especially peracetic acid precursors and pernoanoic acid precursors. Especially preferred bleach DED SHEE~
C6514 (C) WO
Amended 23 January 2001 precursors suitable for use in the present invention are N,N,N',N.-tetracetyl ethylenediamine (TAED) and sodium noanoyloxybenzene sulphonate (SNOBS). The novel quaternary ammonium and phosphonium bleach precursors disclosed in US 4 751 015 and US 4 818 426 (Lever Brothers Company) and EP 402 971A (Unilever), and the cationic bleach precursors disclosed in EP 284 292A and EP 303 520A (Kao) are also of interest.
The bleach system can be either supplemented with or replaced by a peroxyacid. Examples of such peracids can be found in US 4 686 063 and US 5 397 501 (Unilever). A
preferred example is the imido peroxycarboxylic class of peracids described in EP A 325 288, EP A 349 940, DE 382 3172 and EP 325 289. A particularly preferred example is phtalimido peroxy caproic acid (PAP). Such peracids are suitably present at 0.1 - 12%, preferably 0.5 -10%.
A bleach stabiliser (heavy metal sequestrant) may also be present. Suitable bleach stabilisers include ethylenediamine tetra-acetate (EDTA), the polyphosphonates such as Dequest (Trade Mark) and non-phosphate stabilisers such as EDDS (ethylene diamine di-succinic acid). These bleach stabilisers are also useful for stain removal especially in products containing low levels of bleaching species or no bleaching species.
An especially preferred bleach system comprises a peroxy bleach compound (preferably sodium percarbonate optionally ANENDED SHEET
C6514 (C) WO
Amended 23 January 2001 together with a bleach activator), and a transition metal bleach catalyst as described and claimed in EP 458 397A,.
EP 458 398A and EP 50-9 787A (Unilever).
Formulations according to the invention may also contain one or more enzyme(s). Suitable enzymes include the proteases, amylases, cellulases, oxidases, peroxidases and lipases usable for incorporation in detergent compositions.
Preferred proteolytic enzymes (proteases) are, catalytically active protein materials which degrade or alter protein types of stains when pre,sent as in fabric stains in a hydrolysis reaction. They may be of any suitable origin, such as vegetable, animal, bacterial or yeast origin.
Proteolytic enzymes or proteases of various qualities and origins and'having activity in various pH ranges of from.4-12 are available and can be used in the instant invention.
Examples of suitable proteolytic enzymes are the stabilisins which are obtained from particular strains of B. Subtilis B.
licheniformis, such as the commercially available subtilisins Maxatase (Trade Mark), as supplied by Gist Brocades N.V., Delft, Holland, and Alcalase (Trade Mark), as supplied by Novo Industri A/S, Copenhagen, Denmark.
Particularly suitable is a protease obtained from a strain of Bacillus having maximum activity throughout the pH range of 8-12, being commercially available, e.g. from Novo Industri A/S under the registered trade-names Esperase =(Trade Mark) and Savinase (Trade-Mark). The preparation of these and analogous enzymes is described in GB 1 243 785.
Other commercial proteases are Kazusase (Trade Mark AMENDED SNEET
C6514 (C) WO
Amended 23 January 2001 obtainable from Showa-Denko of Japan), Optimase (Trade Mark from Miles Kali-Chemie, Hannover, West Germany), and Superase (Trade Mark obtainable from Pfizer of U.S.A.).
Detergency enzymes are commonly employed in granular form in amounts of from about 0.1 to about 3.0 wt%. However, any suitable physical form of enzyme may be used.
Other materials that may be present in detergent formulations of the invention include sodium silicate;
antiredeposition agents such as cellulosic polymers;
inorganic salts such as sodium sulphate; lather control agents or lather boosters as appropriate; proteolytic and lipolytic enzymes; dyes; coloured speckles; perfumes; foam controllers; fluorescers and decoupling polymers. This list is not intended to be exhaustive.
It is often advantageous if soil release polymers are present.
Test Method and Examples Wrinkle reduction was measured by using the American Association of Textile Chemists and Colorists' (AATCC) method #124, Appearance of Fabrics after Repeated Home Laundering. In this method, four cloth types (silk, rayon, cotton, and linen) are washed, dried and stored in a well defined way. The dried cloths are then evaluated for wrinkle content by comparison with wrinkle smoothness replicas which can be purchases from AATCC. Factors such as the light used, the angle of the cloths and replicas to the h;~~ENME D SNEE?
- 16 - ' light, and the background are carefully controlled and described in the method. There are six replicas with values of 1, 2, 3, 3.5, 4, and 5 with 5 being=perfectly smooth and 1 being very wrinkled. Three trained observers a're asked to give a value.of 1-5, to the nearest 0.5 unit, to each cloth based on which replica it most closely resembles. The results are totalled and averaged over the three observers for each cloth type. According to the'method, a difference of greater than 0.17 between the results for two products indicates there is a significant difference at the 95%
confidence level. A difference of greater than or equal to 0.25 indicates a significant difference at the 99%
confidence level.
FXample 1 The following formulation containing a wrinkle reduction ingredient was produced: = -Formulation 1 ingredient Percent in Formula (by weight) Sodium alcohol ethoxy aulphate 11.0 9E0 alcohol ethoxylate 6.0 Sodium linear alkyl benzene sulphonate 6.0 Propylene glycol 4.0 Sorbitol 3.5 Borax" 2.0 Sodium citrate 1.5 =
Silwet L-7622* 1.0 -Protease enzyme 0.25 Lipase enzyme 0.5 Water to 100$
* Wrinkle reduction agent - polyoxyalkylene modified C6514 (C) WO
Amended 23 January 2001 polydimethylsiloxane from Witco Chemical.Co.
Formulation 2(the same as formulation 1 without the wrinkle reduction agent present) was also produced.
One wash with each detergerit was performed using 111.4g of detergent in 17 gallons (77.27 litres) of water at 95F
(35 C). In each wash, cotton swatches were included along =
with six pounds (2.72 kg)of cotton ballast. The cotton swatches were used to determine the level of wrinkle reduction.
Wrinkle reduction results gave a wrinkle score of 1.78 for the L-7622-containing detergent and 1.17 for the control.
These results indicate a statistical win for the detergent containing L-7622 at the 99% confidence level.
Example 2 The following formulation containing a wrinkle reduction ingredient was produced:
AM~f <~~~ SHEET
Formulation 3 Ingredient Percent in Formula Sodium alcohol ethoxy sulphate 11.0 9EO alcohol ethoxylate 6.0 Sodium linear alkyl benzene'sulphonate 6.0 Propylene glycol 4.0 Sorbitol 3.5 Borax 2.0 Sodium citrate 1.5 Freedom Scan-75- 1.0 Protease enzyme 0.25 Lipase enzyme 0.5 Water To 100$
*Wrinkle reduction agent - sulphated canola oil from Freedom Chemical Co.
Fozmulation 4 (the same as formulation 3 without the wrinkle reduction agent present) was also produced.
One wash with each detergent was performed using 111.4g of detergent in 17 gallons (77.27 litres) of water at 95F
(35 C). In each wash, silk swatches were included along with six pounds (2.72 kg) of cotton ballast. The silk swatches were used to determine the level of wrinkle reduction.
Wrinkle reduction results gave a wrinkle score of 2.89 for =15 the Freedom Scano 75-containing detergent and 2.39 for the control.
These results indicate a statistical win for the detergent containing Freedom'Scano-75 at the 99lr confidence level.
C6514 (C) WO
Amended 23 January 2001 The following formulations show preferred ranges of ingredients in accordance with the present disclosure.
Formluations.5 and 7 represent detergents having ethoxylated organosilicone copolymers as the wrinkle reducing agent while formulations 6 and 8 represent detergents having sulphated castor oil as the wrinkle reducing agent., Formulations 9 and 10 represent powdered and tabulated formulations, respectfully.
AMENDED SHEET
C6514 (C) WO
Amended 23 January 2001 Formulation 5 Ingredient - Chemical Name Percent in Formula (Based on 100W
Active Raw) Alcohol Ethoxylate 4.0 - 15.0 Sodium alkyl ethoxy sulphate . 7.0 - 25.0 Alkylbenzene sulphonic acid 4.0 - 15.0 Sodium Hydroxide 0.3 - 2.5 Propylene glycol 2.0 - 10.0 Sorbitol 2.0 - 10.0 Sodium Tetraborate Pentahydrate 2.0 - 10.0 Sodium Citrate Dihydrate 1.5 - 10.0 Ethoxylated Organosilicone 0.5 - 5,.0 Copolymer Coconut Fatty Acid 0.4 - 2.5 Fluorescent Whitening Agent 0.1 - 0.6 Antiredeposition Agent 0.15 - 1.5 Enzyme - Protease 0.15 - 1.5 Enzyme - Lipase 0 - 2.0 Monoethanolamine 0.1 - 1.5 Perfume 0.1 - 1.0 Water to 100%
AMENDED SHEET
C6514. (C) WO
Amended 23 January 2001 Formulation 6 Ingredient - Chemical Name Percent in Formula (Based on 100t Active Raw) Alcohol Ethoxylate 4.0 - 15.0 Sodium Alkyl Ethoxy Sulphate 7.0 - 25.0 Alkylbenzene Sulphonic Acid 4.0 - 15.0 Sodium Hydroxide 0.3 - 2.5 Propylene Glycol 2.0 - 10.0 Sorbitol 2.0 - 10.0 Sodium Tetraborate Pentahydrate 2.0 - 10.0 Sodium Citrate Dihydrate 1.5 - 10.0 Sulphated=Castor Oil 0.5 - 10.0 Coconut Fatty Acid 0.4 - 2.5 Fluorescent Whitening Agent 0.1 - 0.6 Antiredeposition Agent 0.15 - 1.5 Enzyme - Protease 0.15 - 1.5 Enzyme - Lipase 0 - 2.0 Monoethanolamine 0.1 - 1.5 Perfume 0.1 - 1.0 Water to 100%
AN~D 4 D4p SriEET
C6514 (C) WO
Amended 23 January 2001 Formulation 7 Ingredient - Chemical Name Percent in Formula (Based on 100%
Active Raw) Alcohol Ethoxylate 3.5 - 20.0 Alkylbenzene Sulphonic Acid 9.5 - 30.0 Sodium Hydroxide 1.0 - 10.0 Ethoxylated Organosilicone 0.5 - 5.0 Copolymer Sodium Xylene Siulphonate 0.75 - 10.0 Stearic Acid 0.09 - 0.5 Sodium Silicate 2.0 - 12.0 Fluorescent Whitening Agent 0.04 - 0.4 Perfume 0.1 - 1.0 Water to 100~
Formulation 8 Ingredient - Chemical Name Percent in Formula (Based on 100%
Active Raw) Alcohol Ethoxylate 3.5 - 20.0 Alkylbenzene Sulphonic Acid 9.5 - 30.0 Sodium Hydroxide 1.0 - 10.0 Sulphated Castor Oil 0.5 - 10.0 Sodium Xylene Sulphonate 0.75 - 10.0 Stearic Acid 0.09 - 0.5 Sodium Silicate 2.0 - 12.0 Fluorescent Whitening Agent 0.04 - 0.4 Perfume 0.1 - 1.0 Water to 100t AMENIDED SHEET
C6514 (C) WO
Amended 23 January 2001 Formulation 9 (Detergent Powder) Linear alkylbenzene sulphonate 13.8%
(LAS) Ethoxylated nonionics (5 to 15 5.2%
moles EO) Sodium aluminosilicate 28%
Sodium carbonate 20%
Sodium sulphate 1896 Sodium silicate 0.5%
Polyacrylates 1.4 Sodium perborate 0 to 8%
Protease enzyme 0.5%
Perfume 0.4%
Fluorescent Whitener 0.3%
Anti-Wrinkle agent See Table A
Water and miscellaneous To 100%
AMENDED SNE.F1 C6514 (C) WO
Amended 23 January 2001 Formulation 10 (Detergent Tablet) Linear alkylbenzene sulphonate 9.4%
Ethoxylated nonionics (5 to 15 mole 4%
EO) Sodium aluminosilicate 254k Sodium carbonate 24.5$
Sodium sulphate 5.4%
Sodium Acetate trihydrate 2596 Fluorescent Whitener 0.316 Stearic soap 0.75%
Perfume 0.4%
Protease enzyme 0.5%
Polyacrylates 1.2%
Anti-wrinkle ingredients See Table A
Water and miscellaneous To 100%
Table A (Anti-wrinkle Ingredients) Ethoxylated organosilicones 1-10%
Polyalkyleneoxide modified 1-10%
polydimethylsiloxane Linear aminopolydimethylsiloxane 1-10%
polyalkyeneoxides Sulphated oil 1-10%
Components in Table A can either be used individually or in combination with the total level being preferably between 1 to 10%.
While the above-identified wrinkle reducing agents are preferably incorporated in detergent compositions, they can also be used in other formulations, such as in rinse treatments or other garment care products.
A,~AEt+D~D SHEET
C6514 (C) WO
Amended 23 January 2001 All component percentages are based on weight, unless otherwise indicated. All numerical values are considered to be modified by the term "about" and should be given the broadest available range of equivalents when construing the claims.
AiA~P1~;~ D S~~~C?
Claims (8)
1. A powdered or table detergent formulation comprising a wrinkle reducing agent selected from one or more of sulphated vegetable oils and sulphonated vegetable oils; said laundry detergent formulation comprising from 15 to 60 wt% of surfactant.
2. A formulation according to claim 1, wherein the wrinkle reducing agent comprises a sulphated vegetable oil.
3. A formulation according to claim 2, wherein the sulphated vegetable oil comprises sulphated castor oil.
4. A formulation according to claim 2, wherein the sulphated vegetable oil comprises sulphated canola oil.
5. A formulation according to any one of claims 1 to 4, wherein the wrinkle reducing agent is present in the formulation in an amount from 0.1 wt% to 10 wt%, of the formulation.
6. A formulation according to claim 5, wherein the wrinkle reducing agent is present in the formulation in an amount from 0.1 wt% to 5 wt%.
7. A formulation according to claim 6, wherein the wrinkle reducing agent is present in the formulation in an amount of more preferred limitation from 0.3 wt%
to 1.5 wt %.
to 1.5 wt %.
8. A method of reducing the occurrence of wrinkles in laundered clothing comprising:
providing a detergent formulation according to any one of claims 1 to 5;
contacting the detergent formulation with the clothing during a washing procedure; and allowing the clothing to dry.
providing a detergent formulation according to any one of claims 1 to 5;
contacting the detergent formulation with the clothing during a washing procedure; and allowing the clothing to dry.
Applications Claiming Priority (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10586598P | 1998-10-27 | 1998-10-27 | |
US60/105,865 | 1998-10-27 | ||
US09/293,754 US6403548B1 (en) | 1998-10-27 | 1999-04-16 | Wrinkle reduction laundry product compositions |
US09/293,754 | 1999-04-16 | ||
US09/393,831 | 1999-09-10 | ||
US09/393,831 US6426328B2 (en) | 1998-10-27 | 1999-09-10 | Wrinkle reduction laundry product compositions |
PCT/EP1999/008319 WO2000024857A2 (en) | 1998-10-27 | 1999-10-21 | Wrinkle reduction laundry product compositions |
Publications (2)
Publication Number | Publication Date |
---|---|
CA2347861A1 CA2347861A1 (en) | 2000-05-04 |
CA2347861C true CA2347861C (en) | 2009-01-06 |
Family
ID=27379988
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA002347861A Expired - Fee Related CA2347861C (en) | 1998-10-27 | 1999-10-21 | Wrinkle reduction laundry product compositions |
Country Status (9)
Country | Link |
---|---|
US (2) | US6426328B2 (en) |
EP (1) | EP1124926B1 (en) |
AT (1) | ATE294848T1 (en) |
AU (1) | AU1377900A (en) |
BR (1) | BR9914836B1 (en) |
CA (1) | CA2347861C (en) |
DE (1) | DE69925147T2 (en) |
ES (1) | ES2241370T3 (en) |
WO (1) | WO2000024857A2 (en) |
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-
1999
- 1999-09-10 US US09/393,831 patent/US6426328B2/en not_active Expired - Fee Related
- 1999-10-21 ES ES99971024T patent/ES2241370T3/en not_active Expired - Lifetime
- 1999-10-21 AT AT99971024T patent/ATE294848T1/en not_active IP Right Cessation
- 1999-10-21 AU AU13779/00A patent/AU1377900A/en not_active Abandoned
- 1999-10-21 BR BRPI9914836-6A patent/BR9914836B1/en not_active IP Right Cessation
- 1999-10-21 DE DE69925147T patent/DE69925147T2/en not_active Expired - Lifetime
- 1999-10-21 WO PCT/EP1999/008319 patent/WO2000024857A2/en active IP Right Grant
- 1999-10-21 CA CA002347861A patent/CA2347861C/en not_active Expired - Fee Related
- 1999-10-21 EP EP99971024A patent/EP1124926B1/en not_active Expired - Lifetime
-
2002
- 2002-05-16 US US10/146,732 patent/US6759379B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
EP1124926A2 (en) | 2001-08-22 |
ES2241370T3 (en) | 2005-10-16 |
AU1377900A (en) | 2000-05-15 |
US6426328B2 (en) | 2002-07-30 |
US20010056059A1 (en) | 2001-12-27 |
BR9914836A (en) | 2001-07-10 |
US20020193276A1 (en) | 2002-12-19 |
DE69925147T2 (en) | 2006-02-16 |
CA2347861A1 (en) | 2000-05-04 |
WO2000024857A2 (en) | 2000-05-04 |
BR9914836B1 (en) | 2008-11-18 |
EP1124926B1 (en) | 2005-05-04 |
DE69925147D1 (en) | 2005-06-09 |
ATE294848T1 (en) | 2005-05-15 |
WO2000024857A3 (en) | 2000-08-03 |
US6759379B2 (en) | 2004-07-06 |
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