EP0017120B2 - Textile detergent acting as a finishing agent - Google Patents
Textile detergent acting as a finishing agent Download PDFInfo
- Publication number
- EP0017120B2 EP0017120B2 EP80101534A EP80101534A EP0017120B2 EP 0017120 B2 EP0017120 B2 EP 0017120B2 EP 80101534 A EP80101534 A EP 80101534A EP 80101534 A EP80101534 A EP 80101534A EP 0017120 B2 EP0017120 B2 EP 0017120B2
- Authority
- EP
- European Patent Office
- Prior art keywords
- agent
- content
- ethers
- salts
- quaternary ammonium
- 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
Links
- 239000003599 detergent Substances 0.000 title claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 title claims description 11
- 239000004753 textile Substances 0.000 title abstract description 13
- -1 polysaccharide amino ethers Chemical class 0.000 claims abstract description 18
- 150000003839 salts Chemical class 0.000 claims abstract description 18
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 10
- 239000005017 polysaccharide Substances 0.000 claims abstract description 10
- 125000001453 quaternary ammonium group Chemical group 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims description 12
- 150000002170 ethers Chemical class 0.000 claims description 10
- 125000001033 ether group Chemical group 0.000 claims description 9
- 229920002472 Starch Polymers 0.000 claims description 8
- 239000002736 nonionic surfactant Substances 0.000 claims description 8
- 239000008107 starch Substances 0.000 claims description 8
- 235000019698 starch Nutrition 0.000 claims description 8
- 238000006467 substitution reaction Methods 0.000 claims description 7
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910001424 calcium ion Inorganic materials 0.000 claims description 4
- 150000004676 glycans Chemical class 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 2
- TWNIBLMWSKIRAT-VFUOTHLCSA-N levoglucosan Chemical group O[C@@H]1[C@@H](O)[C@H](O)[C@H]2CO[C@@H]1O2 TWNIBLMWSKIRAT-VFUOTHLCSA-N 0.000 claims description 2
- SBOJXQVPLKSXOG-UHFFFAOYSA-N o-amino-hydroxylamine Chemical class NON SBOJXQVPLKSXOG-UHFFFAOYSA-N 0.000 claims description 2
- 244000007835 Cyamopsis tetragonoloba Species 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 150000008040 ionic compounds Chemical class 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 10
- 238000011282 treatment Methods 0.000 abstract description 5
- 238000004513 sizing Methods 0.000 abstract 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 239000002253 acid Substances 0.000 description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 150000001298 alcohols Chemical class 0.000 description 7
- 239000007844 bleaching agent Substances 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 125000004432 carbon atom Chemical group C* 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 5
- 150000007513 acids Chemical class 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 239000012190 activator Substances 0.000 description 4
- 238000007046 ethoxylation reaction Methods 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 235000019832 sodium triphosphate Nutrition 0.000 description 4
- JDSQBDGCMUXRBM-UHFFFAOYSA-N 2-[2-(2-butoxypropoxy)propoxy]propan-1-ol Chemical group CCCCOC(C)COC(C)COC(C)CO JDSQBDGCMUXRBM-UHFFFAOYSA-N 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 3
- 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 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical class CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229920003086 cellulose ether Polymers 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
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000003760 tallow Substances 0.000 description 3
- PUVAFTRIIUSGLK-UHFFFAOYSA-M trimethyl(oxiran-2-ylmethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1CO1 PUVAFTRIIUSGLK-UHFFFAOYSA-M 0.000 description 3
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 244000303965 Cyamopsis psoralioides Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical class CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 150000008051 alkyl sulfates Chemical class 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 150000002009 diols Chemical group 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- YDSWCNNOKPMOTP-UHFFFAOYSA-N mellitic acid Chemical compound OC(=O)C1=C(C(O)=O)C(C(O)=O)=C(C(O)=O)C(C(O)=O)=C1C(O)=O YDSWCNNOKPMOTP-UHFFFAOYSA-N 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- XIUCEANTZSXBQQ-UHFFFAOYSA-N (3-chloro-2-hydroxypropyl)-trimethylazanium Chemical class C[N+](C)(C)CC(O)CCl XIUCEANTZSXBQQ-UHFFFAOYSA-N 0.000 description 1
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- CIOXZGOUEYHNBF-UHFFFAOYSA-N (carboxymethoxy)succinic acid Chemical compound OC(=O)COC(C(O)=O)CC(O)=O CIOXZGOUEYHNBF-UHFFFAOYSA-N 0.000 description 1
- CFPOJWPDQWJEMO-UHFFFAOYSA-N 2-(1,2-dicarboxyethoxy)butanedioic acid Chemical compound OC(=O)CC(C(O)=O)OC(C(O)=O)CC(O)=O CFPOJWPDQWJEMO-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- CVLHGLWXLDOELD-UHFFFAOYSA-N 4-(Propan-2-yl)benzenesulfonic acid Chemical class CC(C)C1=CC=C(S(O)(=O)=O)C=C1 CVLHGLWXLDOELD-UHFFFAOYSA-N 0.000 description 1
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical class OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- 101100116570 Caenorhabditis elegans cup-2 gene Proteins 0.000 description 1
- 229920003043 Cellulose fiber Polymers 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
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 101100116572 Drosophila melanogaster Der-1 gene Proteins 0.000 description 1
- 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 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 229920001479 Hydroxyethyl methyl cellulose Polymers 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical class CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- QHUFCAZXADDQDX-UHFFFAOYSA-N OP(=O)OP(O)=O.OCC1=CC=CC=C1 Chemical compound OP(=O)OP(O)=O.OCC1=CC=CC=C1 QHUFCAZXADDQDX-UHFFFAOYSA-N 0.000 description 1
- 239000004435 Oxo alcohol Substances 0.000 description 1
- 102000035195 Peptidases Human genes 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical group CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 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
- 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
- 244000274883 Urtica dioica Species 0.000 description 1
- 235000009108 Urtica dioica Nutrition 0.000 description 1
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 229940045714 alkyl sulfonate alkylating agent Drugs 0.000 description 1
- 150000008052 alkyl sulfonates Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000003625 amylolytic effect Effects 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical group OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000001177 diphosphate Substances 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical class [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003165 hydrotropic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000003893 lactate salts Chemical class 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- MBKDYNNUVRNNRF-UHFFFAOYSA-N medronic acid Chemical compound OP(O)(=O)CP(O)(O)=O MBKDYNNUVRNNRF-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- CXHHBNMLPJOKQD-UHFFFAOYSA-N methyl hydrogen carbonate Chemical group COC(O)=O CXHHBNMLPJOKQD-UHFFFAOYSA-N 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 150000004712 monophosphates Chemical class 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical class OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- UFOIOXZLTXNHQH-UHFFFAOYSA-N oxolane-2,3,4,5-tetracarboxylic acid Chemical compound OC(=O)C1OC(C(O)=O)C(C(O)=O)C1C(O)=O UFOIOXZLTXNHQH-UHFFFAOYSA-N 0.000 description 1
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 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
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002797 proteolythic effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000015424 sodium Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000012418 sodium perborate tetrahydrate Substances 0.000 description 1
- 229940045872 sodium percarbonate Drugs 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 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
- 238000001694 spray drying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000001226 triphosphate Substances 0.000 description 1
- 229940006302 tripolyphosphate ion Drugs 0.000 description 1
- 150000004043 trisaccharides Chemical group 0.000 description 1
- 239000008096 xylene Chemical class 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
- C11D3/20—Organic compounds containing oxygen
- C11D3/22—Carbohydrates or derivatives thereof
- C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
- C11D3/227—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin with nitrogen-containing groups
-
- 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
- C11D3/20—Organic compounds containing oxygen
- C11D3/22—Carbohydrates or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
Definitions
- the invention relates to a textile detergent which exerts a finishing or stiffening effect on the washed textiles during the washing process, so that a separate aftertreatment process, usually connected after the last rinse cycle, is unnecessary.
- the detergent-containing textile detergent according to the invention containing a surfactant component and calcium ion-binding skeleton salts, is characterized in that the surfactant component consists of nonionic compounds and that the agent has a content of 0.5 to 10 percent by weight of water-soluble amino ethers of polysaccharides containing quaternary ammonium groups .
- Suitable quaternary groups of ethers of polysaccharides are, in particular, ethers of polygalactomannan and starch.
- polygalctomannan is the main constituent of guar flour and is composed of trisaccharide units with the following structure:
- the ether groups can form on the - CH 2 OH groups, the degree of substitution being in the range from 0.05 to 0.2, preferably from 0.07 to 0.15, ether groups per anhydrogalactomannan unit shown above.
- the degree of substitution for starch ethers is 0.05 to 0.12, preferably 0.07 to 0.1 ether groups per anhydroglucose unit.
- the ether group can be introduced in a manner known per se, for example by reacting the polygalactomannan or starch with ethyleneimine (see US Pat. No. 3,303,184) and then partially or completely quaternizing the amino group.
- ethyleneimine see US Pat. No. 3,303,184
- Such reaction products are described for example in GB-A-1 136842 and are known as additives in papermaking or as flocculants.
- the quaternary salts can be present as halides, in particular chlorides, sulfates, alkyl sulfates, nitrates, phosphates and as salts of organic acids, for example as acetates, citrates or lactates.
- the detergent content of the abovementioned ethers containing quaternary ammonium groups is preferably 1 to 5 percent by weight.
- the textile detergents contain at least one non-ionic surfactant and calcium ion-binding skeleton salts as further constituents. They can also contain conventional detergent components, such as washing alkalis, neutral salts, graying inhibitors, bleaching agents and stabilizers or activators for bleaching agents, enzymes, dyes and fragrances. Compounds with an anionic character which can react with the quaternary polysaccharide aminoethers to form sparingly or insoluble electroneutral salts should not be included in the compositions.
- the content of nonionic surfactants in the laundry detergent is generally 1-30 percent by weight.
- the maximum content is slightly lower in powdery to granular detergents, i.e. it generally does not exceed 25% by weight and is preferably 3-15% by weight.
- Suitable nonionic surfactants are, in particular, ethoxylation products of saturated or monounsaturated aliphatic primary alcohols having 12 to 24, preferably 12 to 18 carbon atoms and 3 to 20, in particular 4 to 15, ethylene glycol ether groups.
- Suitable alcohols from which the present ethoxylation products are derived are, for example, those of natural origin, such as coconut oil or tallow fatty alcohols or oleyl alcohol, furthermore oxo alcohols or synthetic alcohols obtained by ethylene polymerization.
- nonionic surfactants are ethoxylation products of secondary alcohols and vicinal diols, each with 12 to 18 carbon atoms.
- the number of glycol ether groups is also 3 to 20, preferably 4 to 15.
- the abovementioned ethoxylated alcohols and alkylphenols can also be replaced in whole or in part by those which are prepared with 0.5 to 3 moles of propylene oxide per mole of starting compound and only in the second stage the envisaged amount of ethylene oxide is added.
- nonionic surfactants can also be present which are derived from the abovementioned compounds and which have ethylglycol and propylene glycol ether groups in a different order, for example alcohols with 10 to 30 ethylene glycol ether groups and 3 to 30 propylene glycol ether groups; also ethoxylation products of mercaptans, fatty acid amides and fatty acids.
- water-soluble polyethylene oxide adducts containing 20 to 250 ethyl glycol ether groups and 10 to 100 propylene glycol ether groups on polypropylene glycol, ethylene diaminopolypropylene glycol and alkyl polypropylene glycol with 1 to 10 carbon atoms in the alkyl chain.
- the compounds mentioned usually contain 1 to 5 ethylene glycol units per propylene glycol unit.
- Nonionic compounds of the amine oxide and sulfoxide type which can optionally also be ethoxylated, can also be used.
- Suitable structural substances are the polymer phosphates of sodium and potassium.
- the pentasodium triphosphate is particularly suitable as the polymer phosphate, which may be present in a mixture with its hydrolysis products, the mono- and diphosphates, and also more highly condensed phosphates, for example the tetraphosphates.
- These aluminosilicates generally have a grain size of 0.1 to 20 ⁇ m and are preferably crystalline.
- the skeletal salts also include salts of complexing aminopolycarboxylic acids, in particular alkali metal salts of nitrilotriacetic acid and ethylenediaminotetraacetic acid.
- the higher homologues of the aminopolycarboxylic acids mentioned are also suitable.
- Salts of nitrogen-free polycarboxylic acids which form complex salts with calcium ions, including polymers containing carboxyl groups, are also suitable. Examples are citric acid, tartaric acid, benzene hexacarboxylic acid and tetrahydrofuran tetracarboxylic acid.
- Polycarboxylic acids containing carboxymethyl ether groups can also be used, such as 2,2'-oxydisuccinic acid and polyhydric alcohols or hydroxycarboxylic acids partially or completely etherified with glycolic acid, for example triscarboxymethylglycerol, biscarboxymethylglyceric acid and carboxymethyloxysuccinic acid.
- complexing polyphosphonic acid salts can be present, for example the alkali salts of aminopolyphosphonic acids, in particular aminotri- (methylenephosphonic acid), 1-hydroxyethane-1,1-diphosphonic acid, phenylhydroxymethane diphosphonic acid, methylene diphosphonic acid and salts of the higher homologues of the polyphosphonic acid mentioned.
- alkali salts of aminopolyphosphonic acids in particular aminotri- (methylenephosphonic acid), 1-hydroxyethane-1,1-diphosphonic acid, phenylhydroxymethane diphosphonic acid, methylene diphosphonic acid and salts of the higher homologues of the polyphosphonic acid mentioned.
- Mixtures of the aforementioned complexing agents can also be used.
- Suitable washing alkalis are alkali carbonates, bicarbonates, borates and silicates with a Na 2 0: Si0 2 ratio of 1: 1 to 1: 3.5.
- Sodium sulfate and sodium chloride are suitable as neutral salts.
- Suitable graying inhibitors are compounds from the class of cellulose ethers in amounts of 0.1 to 5 percent by weight, in particular nonionic compounds such as methyl cellulose, hydroxyethyl cellulose, methyl hydroxyethyl cellulose and methyl hydroxypropyl cellulose. Mixtures of the aforementioned cellulose ethers or mixed ethers can also be used.
- bleaching agents may be present, preferably per compounds such as sodium percarbonate, but especially sodium perborate tetrahydrate.
- suitable components are foam inhibitors, in particular polydimethylsiloxanes, proteolytic or amylolytic enzymes, and bleach activators, such as tetraacetylethylene diamine or tetraacetylglycoluril.
- the enzymes and bleach activators can be coated with water-soluble or dispersible coating substances.
- the agents can also be in liquid form and contain water or organic solvents, such as low molecular weight alcohols, glycols, glycol ethers and ether alcohols.
- Hydrotropic substances such as the alkali metal salts of toluene, xylene, ethylbenzene and cumene sulfonic acid or alkyl sulfates or alkyl sulfonates having 4 to 8 carbon atoms, may also be present.
- powdered or granular textile detergents can be carried out in a known manner, for example by granulation or spray drying, it being possible for the polysaccharide ethers to be used according to the invention to be added to the detergent pulp to be dusted (slurry).
- the textile detergents are suitable for use in the delicates range (20-40 ° C) and for hot laundry (90-98 ° C), but in particular for the treatment of so-called «easy-care textiles» in the 40-60 ° C range. They are both for washing textiles made of cellulose fibers (cotton, linen) made of refined cellulose (wash-and-wear finish) as well as those made of synthetic fibers or blended fabrics.
- the textile detergents according to the invention are not only distinguished by their high washability but also by valuable finishing and stiffening properties. This manifests itself in an increased bending stiffness and an improved surface smoothness of the washed textiles. These effects are known per se as a result of a finishing treatment, but so far a separate aftertreatment which increases the water consumption and is time-consuming has always been necessary for this purpose. In contrast, the use of the agents according to the invention leads to a simplification of the washing process or to savings in water and energy.
- curtain tape and bleaching nettle were used as textile material.
- the washing treatment was carried out in an automatic washing machine with a horizontally stored drum at 40 ° C ("easy-care program").
- the detergent concentration was 8.4 g / i, the liquor ratio (kg of laundry to liter of wash liquor) 1:20, the water hardness 16 ° dH and the washing time 20 minutes.
- the change in tensile resistance was measured on the curtain tapes, and the change in flexural strength and the static or sliding friction after 1 and 3 washing treatments (abbreviation 1 W and 3 W, respectively).
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Abstract
Description
Gegenstand der Erfindung ist ein Textilwaschmittel, das während des Waschprozesses eine appretierende bzw. steifende Wirkung auf die gewaschenen Textilien ausübt, so dass sich ein gesonderter, meist nach dem letzten Spülgang angeschlossener Nachbehandlungsprozess erübrigt.The invention relates to a textile detergent which exerts a finishing or stiffening effect on the washed textiles during the washing process, so that a separate aftertreatment process, usually connected after the last rinse cycle, is unnecessary.
Das erfindungsgemässe, appretierend wirkende, eine Tensidkomponente und Calciumionen bindende Gerüstsalze enthaltende Textilwaschmittel ist dadurch gekennzeichnet, dass die Tensidkomponente aus nichtionischen Verbindungen besteht und dass das Mittel einen Gehalt von 0,5 bis 10 Gewichtsprozent an in Wasser löslichen, quartären Ammoniumgruppen aufweisenden Aminoethern von Polysacchariden aufweist.The detergent-containing textile detergent according to the invention, containing a surfactant component and calcium ion-binding skeleton salts, is characterized in that the surfactant component consists of nonionic compounds and that the agent has a content of 0.5 to 10 percent by weight of water-soluble amino ethers of polysaccharides containing quaternary ammonium groups .
Als quartäre Gruppen aufweisender Ether von Polysacchariden kommen insbesondere Ether von Polygalactomannan und der Stärke in Frage. Polygalctomannan ist bekanntlich Hauptbestandteil des Guar-Mehls und ist aus Trisaccharid-Einheiten folgender Struktur aufgebaut:
Die Ethergruppen können sich an den - CH2OH-Gruppen ausbilden, wobei der Substitutionsgrad im Bereich von 0,05 bis 0,2, vorzugsweise von 0,07 bis 0,15 Ethergruppen pro vorstehend dargestellter Anhydrogalactomannan-Einheit liegt. Bei den Stärkeethern beträgt der Substitutionsgrad 0,05 bis 0,12, vorzugsweise 0,07 bis 0,1 Ethergruppen pro Anhydroglucose-Einheit.The ether groups can form on the - CH 2 OH groups, the degree of substitution being in the range from 0.05 to 0.2, preferably from 0.07 to 0.15, ether groups per anhydrogalactomannan unit shown above. The degree of substitution for starch ethers is 0.05 to 0.12, preferably 0.07 to 0.1 ether groups per anhydroglucose unit.
Die Einführung der Ethergruppe kann in an sich bekannter Weise, beispielsweise durch Umsetzung des Polygalactomannans beziehungsweise der Stärke mit Ethylenimin (vergleiche US-A-3 303 184) und anschliessende teilweise oder vollständige Quaternierung der Aminogruppe erfolgen. Vorzugsweise werden jedoch solche Ether verwendet, die beispielweise durch Umsetzung von Polygalactomannan beziehungsweise Stärke mit 2,3-Epoxypropyltrialkylammoniumsalzen oder 3-Chlor-2-hydroxypropyltrimethylammoni- umsalzen, insbesondere mit 2,3-Epoxypropyltrimethylammoniumchlorid, erhalten werden. Derartige Umsetzungsprodukte sind beispielsweise in der GB-A-1 136842 beschrieben und sind als Zusätze bei der Papierherstellung beziehungsweise als Flockungsmittel bekannt.The ether group can be introduced in a manner known per se, for example by reacting the polygalactomannan or starch with ethyleneimine (see US Pat. No. 3,303,184) and then partially or completely quaternizing the amino group. However, preference is given to using ethers which are obtained, for example, by reacting polygalactomannan or starch with 2,3-epoxypropyltrialkylammonium salts or 3-chloro-2-hydroxypropyltrimethylammonium salts, in particular with 2,3-epoxypropyltrimethylammonium chloride. Such reaction products are described for example in GB-A-1 136842 and are known as additives in papermaking or as flocculants.
Die Quartärsalze können als Halogenide, insbesondere Chloride, Sulfate, Alkylsulfate, Nitrate, Phosphate und als Salze organischer Säuren, zum Beispiel als Acetate, Citrate oder Lactate vorliegen. Der Gehalt der Waschmittel an den vorgenannten, quartären Ammoniumgruppen aufweisenden Ethern beträgt vorzugsweise 1 bis 5 Gewichtsprozent.The quaternary salts can be present as halides, in particular chlorides, sulfates, alkyl sulfates, nitrates, phosphates and as salts of organic acids, for example as acetates, citrates or lactates. The detergent content of the abovementioned ethers containing quaternary ammonium groups is preferably 1 to 5 percent by weight.
Die Textilwaschmittel enthalten als weitere Bestandteile mindestens ein nichtionisches Tensid sowie Calciumionen bindende Gerüstsalze. Sie können ferner übliche Waschmittelbestandteile, wie Waschalkalien, Neutralsalze, Vergrauungsinhibitoren, Bleichmittel sowie Stabilisatoren beziehungsweise Aktivatoren für Bleichmittel, Enzyme, Farb- und Duftstoffe enthalten. Verbindungen mit anionischem Charakter, die mit den quartären Polysaccharid-Aminoethern unter Bildung schwer- beziehungsweise unlöslicher Elektroneutralsalze reagieren können, sollen in den Mitteln nicht enthalten sein.The textile detergents contain at least one non-ionic surfactant and calcium ion-binding skeleton salts as further constituents. They can also contain conventional detergent components, such as washing alkalis, neutral salts, graying inhibitors, bleaching agents and stabilizers or activators for bleaching agents, enzymes, dyes and fragrances. Compounds with an anionic character which can react with the quaternary polysaccharide aminoethers to form sparingly or insoluble electroneutral salts should not be included in the compositions.
Der Gehalt der Textilwaschmittel an nichtionischen Tensiden beträgt allgemein 1-30 Gewichtsprozent. In pulverförmigen bis körnigen Waschmitteln ist der maximale Gehalt etwas niedriger, d.h. er übersteigt 25 Gewichtsprozent im allgemeinen nicht und beträgt vorzugsweise 3-15 Gewichtsprozent.The content of nonionic surfactants in the laundry detergent is generally 1-30 percent by weight. The maximum content is slightly lower in powdery to granular detergents, i.e. it generally does not exceed 25% by weight and is preferably 3-15% by weight.
Geeignete nichtionische Tenside sind insbesondere Ethoxylierungsprodukte von gesättigten oder einfach ungesättigten aliphatischen primären Alkoholen mit 12 bis 24, vorzugsweise 12 bis 18 Kohlenstoffatomen und 3 bis 20 insbesondere 4 bis 15 Ethylenglykolethergruppen. Geeignete Alkohole, von denen sich die vorliegenden Ethoxylierungsprodukte ableiten, sind beispielsweise solche natürlichen Ursprungs, wie Cocos- oder Talgfettalkohole bzw. Oleylalkohol, ferner Oxoalkohole oder durch Ethylenpolymerisation gewonnenen Synthesealkohole.Suitable nonionic surfactants are, in particular, ethoxylation products of saturated or monounsaturated aliphatic primary alcohols having 12 to 24, preferably 12 to 18 carbon atoms and 3 to 20, in particular 4 to 15, ethylene glycol ether groups. Suitable alcohols from which the present ethoxylation products are derived are, for example, those of natural origin, such as coconut oil or tallow fatty alcohols or oleyl alcohol, furthermore oxo alcohols or synthetic alcohols obtained by ethylene polymerization.
Weitere geeignete nichtionische Tenside sind Ethoxylierungsprodukte von sekundären Alkoholen und vicinalen Diolen mit jeweils 12 bis 18 Koh-Other suitable nonionic surfactants are ethoxylation products of secondary alcohols and vicinal diols, each with 12 to 18 carbon atoms.
lenstoffatomen sowie von Alkylphenolen mit 6 bis 12 Kohlenstoffatomen im Alkylrest, wobei die Zahl der Glykolethergruppen ebenfalls 3 bis 20, vorzugsweise 4 bis 15 beträgt. Die vorstehend genannten ethoxylierten Alkohole und Alkylphenole können auch ganz oder teilweise durch solche ersetzt sein, bei deren Herstellung mit 0,5 bis 3 Mol Propylenoxid pro Mol Ausgangsverbindung und erst in 2. Stufe die in Aussicht genommene Menge an Ethylenoxid angelagert wird.lenstoffatomen and of alkylphenols with 6 to 12 carbon atoms in the alkyl radical, the number of glycol ether groups is also 3 to 20, preferably 4 to 15. The abovementioned ethoxylated alcohols and alkylphenols can also be replaced in whole or in part by those which are prepared with 0.5 to 3 moles of propylene oxide per mole of starting compound and only in the second stage the envisaged amount of ethylene oxide is added.
Gegebenenfalls können auch solche nichtionischen Tenside anwesend sein, die sich von den vorgenannten Verbindungen ableiten und die Ethylglykol- als auch Propylenglykolethergruppen in anderer Reihenfolge aufweisen, beispielsweise Alkohole mit 10 bis 30 Ethylenglykolethergruppen und 3 bis 30 Propylenglykolethergruppen; ferner Ethoxylierungsprodukte von Mercaptanen, Fettsäureamiden und Fettsäuren. Brauchbar sind auch die wasserlöslichen, 20 bis 250 Ethylglykolethergruppen und 10 bis 100 Propylenglykolethergruppen enthaltenden Polyethylenoxidaddukte an Polypropylenglykol, Ethylendiaminopolypropylenglykol und Alkylpolypropylenglykol mit 1 bis 10 Kohlenstoffatomen in der Alkylkette. Die genannten Verbindungen enthalten üblicherweise pro Propylenglykol-Einheit 1 bis 5 Ethylenglykoleinheiten. Auch nichtionische Verbindungen vom Typ der Aminoxide und Sulfoxide, die gegebenenfalls auch ethoxyliert sein können, sind verwendbar.If appropriate, such nonionic surfactants can also be present which are derived from the abovementioned compounds and which have ethylglycol and propylene glycol ether groups in a different order, for example alcohols with 10 to 30 ethylene glycol ether groups and 3 to 30 propylene glycol ether groups; also ethoxylation products of mercaptans, fatty acid amides and fatty acids. Also usable are the water-soluble polyethylene oxide adducts containing 20 to 250 ethyl glycol ether groups and 10 to 100 propylene glycol ether groups on polypropylene glycol, ethylene diaminopolypropylene glycol and alkyl polypropylene glycol with 1 to 10 carbon atoms in the alkyl chain. The compounds mentioned usually contain 1 to 5 ethylene glycol units per propylene glycol unit. Nonionic compounds of the amine oxide and sulfoxide type, which can optionally also be ethoxylated, can also be used.
Geeignete Gerüstsubstanzen sind die Polymerphosphate des Natriums und Kaliums. Als Polymerphosphat kommt insbesondere das Pentanatriumtriphosphat in Frage, das im Gemisch mit seinen Hydrolyseprodukten, den Mono- und Diphosphaten, sowie höherkondensierten Phosphaten, zum Beispiel den Tetraphosphaten, vorliegen kann. Brauchbar sind ferner zum Kationenaustausch befähigte, wasserhaltige Alumosilikate des Kaliums oder insbesondere des Natriums der allgemeinen Formel
Diese Alumosilikate weisen allgemein eine Korngrösse von 0,1 bis 20 µm auf und sind vorzugsweise kristallin.Suitable structural substances are the polymer phosphates of sodium and potassium. The pentasodium triphosphate is particularly suitable as the polymer phosphate, which may be present in a mixture with its hydrolysis products, the mono- and diphosphates, and also more highly condensed phosphates, for example the tetraphosphates. It is also possible to use water-containing aluminum silicates of potassium or, in particular, sodium of the general formula which are capable of cation exchange
These aluminosilicates generally have a grain size of 0.1 to 20 μm and are preferably crystalline.
Zu den Gerüstsalzen zählen ferner Salze von komplexierend wirkenden Aminopolycarbonsäuren insbesondere Alkalisalze der Nitrilotriessigsäure und Ethylendiaminotetraessigsäure. Geeignet sind ferner die höheren Homologen der genannten Aminopolycarbonsäuren. Auch Salze stickstofffreier, mit Calciumionen Komplexsalze bildender Polycarbonsäuren, wozu auch Carboxylgruppen enthaltende Polymerisate zählen, sind geeignet. Beispiele sind Citronsäure, Weinsäure, Benzolhexacarbonsäure und Tetrahydrofurantetracarbonsäure. Auch Carboxymethylethergruppen enthaltende Polycarbonsäuren sind brauchbar, wie 2,2'-Oxydibemsteinsäure sowie mit Glykolsäure teilweise oder vollständig veretherte mehrwertige Alkohole oder Hydroxycarbonsäuren, beispielsweise Triscarboxymethylglycerin, Biscarboxymethylglycerinsäure und Carboxymethyl-oxybernsteinsäure.The skeletal salts also include salts of complexing aminopolycarboxylic acids, in particular alkali metal salts of nitrilotriacetic acid and ethylenediaminotetraacetic acid. The higher homologues of the aminopolycarboxylic acids mentioned are also suitable. Salts of nitrogen-free polycarboxylic acids which form complex salts with calcium ions, including polymers containing carboxyl groups, are also suitable. Examples are citric acid, tartaric acid, benzene hexacarboxylic acid and tetrahydrofuran tetracarboxylic acid. Polycarboxylic acids containing carboxymethyl ether groups can also be used, such as 2,2'-oxydisuccinic acid and polyhydric alcohols or hydroxycarboxylic acids partially or completely etherified with glycolic acid, for example triscarboxymethylglycerol, biscarboxymethylglyceric acid and carboxymethyloxysuccinic acid.
Weiterhin können komplexierend wirkende polyphosphonsaure Salze anwesend sein, zum Beispiel die Alkalisalze von Aminopolyphosphonsäuren, insbesondere Aminotri-(methylenphosphon- säure), 1 -Hydroxyethan-1,1 -diphosphonsäure, Phenylhydroxymethandiphosphonsäure, Methylendiphosphonsäure sowie Salze der höheren Homologen der genannten Polyphosphonsäure. Auch Gemische der vorgenannten Komplexierungsmittel sind verwendbar.Furthermore, complexing polyphosphonic acid salts can be present, for example the alkali salts of aminopolyphosphonic acids, in particular aminotri- (methylenephosphonic acid), 1-hydroxyethane-1,1-diphosphonic acid, phenylhydroxymethane diphosphonic acid, methylene diphosphonic acid and salts of the higher homologues of the polyphosphonic acid mentioned. Mixtures of the aforementioned complexing agents can also be used.
Geeignete Waschalkalien sind Alkalicarbonate, -bicarbonate, -borate und -silikate mit einem Na20:Si02-Verhältnis von 1:1 bis 1:3,5. Als Neutralsalze kommen Natriumsulfat und Natriumchlorid in Betracht.Suitable washing alkalis are alkali carbonates, bicarbonates, borates and silicates with a Na 2 0: Si0 2 ratio of 1: 1 to 1: 3.5. Sodium sulfate and sodium chloride are suitable as neutral salts.
Als Vergrauungsinhibitoren kommen Verbindungen aus der Klasse der Celluloseether in Mengen von 0,1 bis 5 Gewichtsprozent in Betracht, insbesondere nichtionische Verbindungen, wie Methylcellulose, Hydroxyethylcellulose, Methylhydroxyethylcellulose und Methyl-hydroxypropylcellulose. Auch Gemische der vorgenannten Celluloseether beziehungsweise Mischether können eingesetzt werden.Suitable graying inhibitors are compounds from the class of cellulose ethers in amounts of 0.1 to 5 percent by weight, in particular nonionic compounds such as methyl cellulose, hydroxyethyl cellulose, methyl hydroxyethyl cellulose and methyl hydroxypropyl cellulose. Mixtures of the aforementioned cellulose ethers or mixed ethers can also be used.
Gegebenfalls können Bleichmittel anwesend sein, vorzugsweise Perverbindungen, wie Natriumpercarbonat, insbesondere jedoch Natriumperborat-tetrahydrat. Weitere geeignete Bestandteile sind Schauminhibitoren, insbesondere Polydimethylsiloxane, proteolytische beziehungsweise am amylolytische Enzyme sowie Bleichaktivatoren, wie Tetraacetylethylendiamin oder Tetraacetylglykoluril. Zum Schutz gegen Zersetzung oder Wechselwirkungen mit den übrigen Pulverbestandteilen des Waschmittels können die Enzyme und Bleichaktivatoren mit in Wasser löslichen beziehungsweise dispergierbaren Hüllsubstanzen überzogen sein.If necessary, bleaching agents may be present, preferably per compounds such as sodium percarbonate, but especially sodium perborate tetrahydrate. Other suitable components are foam inhibitors, in particular polydimethylsiloxanes, proteolytic or amylolytic enzymes, and bleach activators, such as tetraacetylethylene diamine or tetraacetylglycoluril. To protect against decomposition or interactions with the other powder components of the detergent, the enzymes and bleach activators can be coated with water-soluble or dispersible coating substances.
Die Mittel können auch in flüssiger Form vorliegen und Wasser beziehungsweise organische Lösungsmittel, wie niedermolekulare Alkohole, Glykole, Glykolether und Etheralkohole enthalten. Ebenso können hydrotrope Stoffe, wie die Alkalimetallsalze der Toluol-, Xylol-, Ethylbenzol-und Cumolsulfonsäure beziehungsweise Alkylsulfate oder Alkylsulfonate mit4 bis 8 Kohlenstoffatomen anwesend sein.The agents can also be in liquid form and contain water or organic solvents, such as low molecular weight alcohols, glycols, glycol ethers and ether alcohols. Hydrotropic substances, such as the alkali metal salts of toluene, xylene, ethylbenzene and cumene sulfonic acid or alkyl sulfates or alkyl sulfonates having 4 to 8 carbon atoms, may also be present.
Die Herstellung pulverförmiger beziehungsweise körnigertextilwaschmittel kann in bekannter Weise durchgeführt werden, beispielsweise durch Granulation oder Sprühtrocknung, wobei die erfindungsgemäss mitzuverwendenden Polysaccharidether dem zu verstäubenden Waschmittelbrei (Slurry) zugesetzt werden können.The production of powdered or granular textile detergents can be carried out in a known manner, for example by granulation or spray drying, it being possible for the polysaccharide ethers to be used according to the invention to be added to the detergent pulp to be dusted (slurry).
Die Textilwaschmittel eignen sich zur Verwendung im Feinwaschbereich (20-40°C) und für Kochwäsche (90-98°C), insbesondere jedoch zur Behandlung von sogenannten «Pflegeleicht-Textilien» im 40-60°C-Waschbereich. Sie sind sowohl zum Waschen von Textilien aus Cellulosefasern (Baumwolle, Leinen) aus veredelter Cellulose (wash-and-wear-Ausrüstung) als auch .von solchen aus Synthesefasern beziehungsweise Mischgeweben geeignet.The textile detergents are suitable for use in the delicates range (20-40 ° C) and for hot laundry (90-98 ° C), but in particular for the treatment of so-called «easy-care textiles» in the 40-60 ° C range. They are both for washing textiles made of cellulose fibers (cotton, linen) made of refined cellulose (wash-and-wear finish) as well as those made of synthetic fibers or blended fabrics.
Pulverförmige bis körnige Waschmittel können folgende allgemeine Zusammensetzung aufweisen (in Gewichtsprozent):
- 0,5-10%, vorzugsweise 1-5% der quartären Ammoniumgruppen aufweisenden Polysaccharidether,
- 1-25%, vorzugsweise 3-15% an nichtionischen Tensiden, insbesondere ethoxylierten Alkoholen,
- 10-60%, vorzugsweise 25-50% an Gerüstsalzen, insbesondereTripolyphosphatund/oderCaleiumionen bindenden Alumosilikaten,
- 0-25%, vorzugsweise 1-15% an Waschalkalien, insbesondere Natriumsilikat und/oder Natriumcarbonat,
- 0-4%, vorzugsweise 0,5-2% an Vergrauungsinhibitoren, insbesondere nichtionischen Celluloseethern,
- 0-30% an Bleichmitteln sowie deren Kombination mit Bleichaktivatoren und Stabilisatoren, vorzugsweise 10 bis 25% Perborat,
- 0-4%, vorzugsweise 0,1-2,5% an Magnesiumsilikat und/oder Ethylendiaminotetraacetat als Perboratstabilisatoren,
- 0-30% an sonstigen Waschmittelbestandteilen einschliesslich Natriumsulfat.
- 0.5-10%, preferably 1-5% of the polysaccharide ethers containing quaternary ammonium groups,
- 1-25%, preferably 3-15% of nonionic surfactants, especially ethoxylated alcohols,
- 10-60%, preferably 25-50% of framework salts, in particular tripolyphosphate and / or potassium ion-binding aluminosilicates,
- 0-25%, preferably 1-15% of washing alkalis, especially sodium silicate and / or sodium carbonate,
- 0-4%, preferably 0.5-2%, of graying inhibitors, in particular nonionic cellulose ethers,
- 0-30% of bleaching agents and their combination with bleach activators and stabilizers, preferably 10 to 25% perborate,
- 0-4%, preferably 0.1-2.5%, of magnesium silicate and / or ethylenediaminotetraacetate as perborate stabilizers,
- 0-30% of other detergent ingredients including sodium sulfate.
Flüssige Textilwaschmittel können die folgende Zusammensetzung aufweisen (in Gewichtsprozent):
- 0,5-5%, vorzugsweise 1 bis 5% der quartären Ammoniumgruppen aufweisenden Polysaccharidether,
- 3-30%, vorzugsweise 5 bis 25% an nichtionischen Tensiden, insbesondere ethoxylierten Alkoholen,
- 0-20% an wasserlöslichen Gerüstsalzen, insbesondere Natrium- oder Kaliumphosphat beziehungsweise-tripolyphosphat,
- 0-2% an Sequestrierungsmitteln, insbesondere Na-Ethylendiaminotetraacetat
- 2-20% an organischen Lösungsmitteln aus der Klasse der 1 bis 3 C-Atome pro Alkoholrest aufweisenden Monoalkohole, Diole, Etheralkohole und Glykolether,
- 0-1% an Farb-, Duft- und Konservierungsstoffen,
Rest Wasser.Liquid laundry detergents can have the following composition (in percent by weight):
- 0.5-5%, preferably 1 to 5% of the quaternary ammonium polysaccharide ethers,
- 3-30%, preferably 5 to 25% of nonionic surfactants, especially ethoxylated alcohols,
- 0-20% of water-soluble skeletal salts, in particular sodium or potassium phosphate or tripolyphosphate,
- 0-2% of sequestering agents, especially Na ethylenediaminotetraacetate
- 2-20% of organic solvents from the class of 1 to 3 carbon atoms per alcohol residue-containing monoalcohols, diols, ether alcohols and glycol ethers,
- 0-1% of colors, fragrances and preservatives,
Rest of water.
Die erfindungsgemässen Textilwaschmittel zeichnen sich ausser durch ihr hohes Waschvermögen auch durch wertvolle appretierende und steifende Eigenschaften aus. Dies äussert sich in einer erhöhten Biegesteifigkeit und einer verbesserten Oberflächenglätte der gewaschenen Textilien. An sich sind diese Effekte als Folgen einer Appretierbehandlung bekannt, nur war hierzu bisher stets eine gesonderte, den Wasserverbrauch erhöhende und zeitlich aufwendigere Nachbehandlung erforderlich. Die Anwendung der erfindungsgemässen Mittel führt demgegenüber zu einer Vereinfachung des Waschprozesses beziehungsweise zu Einsparungen an Wasser und Energie.The textile detergents according to the invention are not only distinguished by their high washability but also by valuable finishing and stiffening properties. This manifests itself in an increased bending stiffness and an improved surface smoothness of the washed textiles. These effects are known per se as a result of a finishing treatment, but so far a separate aftertreatment which increases the water consumption and is time-consuming has always been necessary for this purpose. In contrast, the use of the agents according to the invention leads to a simplification of the washing process or to savings in water and energy.
Es wurde ein Waschmittel folgender Zusammensetzung verwendet (in Gewichtsprozent):
- 5,0% ethoxylierter Talgalkohol(14EO)
- 3,0% ethoxylierterTalgalkohol(5E0)
- 40,0% Na-Tripolyphosphat
- 6,5% Soda
- 4,5% Natriumsilikat (Na20:Si02=3,3:1 )
- 0,2% Na-Ethylendiaminotetraacetat
- 0,2% proteolytisches Enzym
- 26,6% Natriumsulfat
- 9,5% Wasser
- 5.0% ethoxylated tallow alcohol (14EO)
- 3.0% ethoxylated tallow alcohol (5E0)
- 40.0% Na tripolyphosphate
- 6.5% soda
- 4.5% sodium silicate (Na 2 0: Si0 2 = 3.3: 1)
- 0.2% Na ethylenediamine tetraacetate
- 0.2% proteolytic enzyme
- 26.6% sodium sulfate
- 9.5% water
Der Polysaccharid-Ether bestand aus
- A) Polygalactomannan-ether, hergestellt durch Umsetzung von Guarmehl mit 2,3-Epoxypropyl-trimethylammoniumchlorid, Substitutionsgrad = 0,1 quartäre Ethergruppe pro Anhydrogalactomannan-Einheit,
- B) Polygalactomannan-ether, hergestellt wie Produkt (A), Substitutionsgrad = 0,15 quartäre Ethergruppen pro Anhydrogalactomannan-Einheit,
- C) Stärkeether, hergestellt durch Umsetzung von Stärke mit 2,3-Epoxypropyl-trimethylammoniumchlorid, Substitutionsgrad = 0,085 quartäre Ethergruppen pro Anhydroglycose-Einheit.
- A) polygalactomannan ether, prepared by reacting guar flour with 2,3-epoxypropyltrimethylammonium chloride, degree of substitution = 0.1 quaternary ether group per anhydrogalactomannan unit,
- B) polygalactomannan ether, prepared as product (A), degree of substitution = 0.15 quaternary ether groups per anhydrogalactomannan unit,
- C) Starch ether, produced by reacting starch with 2,3-epoxypropyltrimethylammonium chloride, degree of substitution = 0.085 quaternary ether groups per anhydroglycose unit.
Im Vergleichsversuch wurde der Polysaccharid-ether durch Natriumsulfat ersetzt.In the comparative experiment, the polysaccharide ether was replaced by sodium sulfate.
Als Textilmaterial wurde Gardinenband und Bleichnessel verwendet. Die Waschbehandlung erfolgte in einer automatischen Waschmaschine mit horizontal gelagerter Trommel bei 40°C («Pflegeleicht-Programm»). Die Waschmittelkonzentration betrug 8,4 g/i, das Flottenverhältnis (kg Wäsche zu Liter Waschlauge) 1:20, die Wasserhärte 16° dH und die Waschdauer 20 Minuten. Nach Entfernung der Waschlauge wurde dreimal mit Wasser nachgespült und getrocknet. An den Gardinenbändern wurde die Veränderung des Zugwiderstandes, am Nesselgewebe die der Biegefestigkeit und der Haft- beziehungsweise Gleitreibung nach jeweils 1 und 3 Waschbehandlungen (Abkürzung 1 W beziehungsweise 3 W) gemessen. Eine Erhöhung des Zugwiderstandes und der Biegefestigkeit entspricht einer Gebrauchswerterhöhung; eine Erniedrigung der Haftreibung und Gleitreibung entspricht einer (erwünschten) Verbesserung der Oberflächenglätte. Die in der folgenden Tabelle aufgeführten Testergebnisse (angegeben in cN) belegen die Überlegenheit der erfindungsgemässen Mittel.Curtain tape and bleaching nettle were used as textile material. The washing treatment was carried out in an automatic washing machine with a horizontally stored drum at 40 ° C ("easy-care program"). The detergent concentration was 8.4 g / i, the liquor ratio (kg of laundry to liter of wash liquor) 1:20, the water hardness 16 ° dH and the washing time 20 minutes. After the wash liquor had been removed, it was rinsed three times with water and dried. The change in tensile resistance was measured on the curtain tapes, and the change in flexural strength and the static or sliding friction after 1 and 3 washing treatments (abbreviation 1 W and 3 W, respectively). An increase in tensile resistance and flexural strength corresponds to an increase in use value; a reduction in static friction and sliding friction corresponds to a (desired) improvement in surface smoothness. The test results listed in the following table (given in cN) demonstrate the superiority of the agents according to the invention.
An Babywindeln aus veredelter Baumwolle, die in der gleichen Weise bei einer Waschtemperatur von 60°C gewaschen wurden, war eine deutliche Abnahme der Oberflächenreibung bzw. der Haftreibung festzustellen.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT80101534T ATE1248T1 (en) | 1979-03-26 | 1980-03-24 | FINISHING TEXTILE DETERGENT. |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19792911857 DE2911857A1 (en) | 1979-03-26 | 1979-03-26 | APPEARING TEXTILE DETERGENT |
| DE2911857 | 1979-03-26 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP0017120A1 EP0017120A1 (en) | 1980-10-15 |
| EP0017120B1 EP0017120B1 (en) | 1982-06-23 |
| EP0017120B2 true EP0017120B2 (en) | 1985-09-04 |
Family
ID=6066464
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP80101534A Expired EP0017120B2 (en) | 1979-03-26 | 1980-03-24 | Textile detergent acting as a finishing agent |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US4289642A (en) |
| EP (1) | EP0017120B2 (en) |
| AT (1) | ATE1248T1 (en) |
| BR (1) | BR8001788A (en) |
| DE (2) | DE2911857A1 (en) |
| DK (1) | DK89880A (en) |
| ZA (1) | ZA801721B (en) |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8334159D0 (en) * | 1983-12-22 | 1984-02-01 | Unilever Plc | Perfume |
| DE3542725A1 (en) * | 1985-12-03 | 1987-06-04 | Hoffmann Staerkefabriken Ag | LAUNDRY TREATMENT AGENT |
| DE3842007A1 (en) * | 1988-12-14 | 1990-06-21 | Henkel Kgaa | FLUID TO PASTOESES, BLEACHING DETERGENT |
| US5150312A (en) * | 1989-06-16 | 1992-09-22 | International Business Machines Corporation | Animation processor method and apparatus |
| DE4301459A1 (en) * | 1993-01-20 | 1994-07-21 | Huels Chemische Werke Ag | Aqueous fabric softener for the treatment of textiles |
| DE4411681A1 (en) * | 1994-04-05 | 1995-10-12 | Hoechst Ag | Process for the preparation of low molecular weight polysaccharide ethers |
| US5851971A (en) * | 1997-09-25 | 1998-12-22 | Colgate-Palmolive Company | Liquid cleaning compositions |
| US6180582B1 (en) * | 1997-09-26 | 2001-01-30 | Colgate-Palmolive Co. | Liquid cleaning compositions |
| GB2342358A (en) * | 1998-10-09 | 2000-04-12 | Procter & Gamble | Detergent compositions comprising cationic polymers |
| US6281172B1 (en) | 1999-04-07 | 2001-08-28 | Akzo Nobel Nv | Quaternary nitrogen containing amphoteric water soluble polymers and their use in drilling fluids |
| WO2001030951A1 (en) * | 1999-10-22 | 2001-05-03 | Reckitt Benckiser France | Compositions and their use |
| US6849586B2 (en) | 2001-10-26 | 2005-02-01 | S. C. Johnson & Son, Inc. | Hard surface cleaners containing chitosan |
| DE102004021732A1 (en) | 2004-04-30 | 2005-11-24 | Henkel Kgaa | Textilplegemittel with amine group-containing cellulose ether |
| US20060217287A1 (en) * | 2005-03-22 | 2006-09-28 | Unilever Home & Personal Care Usa, Division Of Conopco, Inc. | Fabric softening composition |
| US20060223739A1 (en) * | 2005-04-05 | 2006-10-05 | Unilever Home And Personal Care Usa, Division Of Conopco, Inc. | Fabric softening composition with cationic polymer, soap, and amphoteric surfactant |
| DE102007036394A1 (en) * | 2007-07-31 | 2009-02-05 | Henkel Ag & Co. Kgaa | Textile care agent with amine group-containing cellulose ether |
| US10273434B2 (en) * | 2010-06-18 | 2019-04-30 | Rhodia Operations | Protection of the color of textile fibers by means of cationic polysacchrides |
| FR2961522B1 (en) * | 2010-06-18 | 2013-03-15 | Rhodia Operations | PROTECTION OF THE COLORING OF TEXTILE FIBERS BY CATIONIC POLYSACCHARIDES |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3753916A (en) * | 1967-09-27 | 1973-08-21 | Procter & Gamble | Detergent compositions containing particle deposition enhancing agents |
| US3580853A (en) * | 1967-09-27 | 1971-05-25 | Procter & Gamble | Detergent compositions containing particle deposition enhancing agents |
| US3990991A (en) * | 1974-02-01 | 1976-11-09 | Revlon, Inc. | Shampoo conditioner formulations |
| US4031307A (en) * | 1976-05-03 | 1977-06-21 | Celanese Corporation | Cationic polygalactomannan compositions |
| US4061602A (en) * | 1976-08-03 | 1977-12-06 | American Cyanamid Company | Conditioning shampoo composition containing a cationic derivative of a natural gum (such as guar) as the active conditioning ingredient |
| DE2658575A1 (en) * | 1976-12-23 | 1978-06-29 | Henkel Kgaa | Rinsing compsn. with stiffening and brightening effect - contg. quat. ammonium salt and vinyl! copolymer with free carboxy gps. |
| US4179382A (en) * | 1977-11-21 | 1979-12-18 | The Procter & Gamble Company | Textile conditioning compositions containing polymeric cationic materials |
| US4169945A (en) * | 1978-01-05 | 1979-10-02 | Celanese Corporation | Process for production of polygalactomannan ethers |
-
1979
- 1979-03-26 DE DE19792911857 patent/DE2911857A1/en not_active Withdrawn
-
1980
- 1980-02-29 US US06/126,037 patent/US4289642A/en not_active Expired - Lifetime
- 1980-03-03 DK DK89880A patent/DK89880A/en not_active Application Discontinuation
- 1980-03-24 DE DE8080101534T patent/DE3060571D1/en not_active Expired
- 1980-03-24 ZA ZA00801721A patent/ZA801721B/en unknown
- 1980-03-24 EP EP80101534A patent/EP0017120B2/en not_active Expired
- 1980-03-24 AT AT80101534T patent/ATE1248T1/en not_active IP Right Cessation
- 1980-03-25 BR BR8001788A patent/BR8001788A/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| DE3060571D1 (en) | 1982-08-12 |
| DK89880A (en) | 1980-09-27 |
| DE2911857A1 (en) | 1980-10-16 |
| ZA801721B (en) | 1981-06-24 |
| EP0017120B1 (en) | 1982-06-23 |
| EP0017120A1 (en) | 1980-10-15 |
| BR8001788A (en) | 1980-11-18 |
| US4289642A (en) | 1981-09-15 |
| ATE1248T1 (en) | 1982-07-15 |
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