DK160886B - Et beskyttet enzymsystem og en flydende rensemiddelsammensaetning indeholdende dette - Google Patents
Et beskyttet enzymsystem og en flydende rensemiddelsammensaetning indeholdende dette Download PDFInfo
- Publication number
- DK160886B DK160886B DK086187A DK86187A DK160886B DK 160886 B DK160886 B DK 160886B DK 086187 A DK086187 A DK 086187A DK 86187 A DK86187 A DK 86187A DK 160886 B DK160886 B DK 160886B
- Authority
- DK
- Denmark
- Prior art keywords
- enzyme
- liquid
- dispersed
- sodium
- pascal seconds
- Prior art date
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- 102000004190 Enzymes Human genes 0.000 title claims description 89
- 108090000790 Enzymes Proteins 0.000 title claims description 89
- 239000000203 mixture Substances 0.000 title claims description 63
- 239000007788 liquid Substances 0.000 title claims description 50
- 238000004140 cleaning Methods 0.000 title description 4
- 239000003599 detergent Substances 0.000 claims description 50
- 230000002209 hydrophobic effect Effects 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 239000004094 surface-active agent Substances 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 239000012141 concentrate Substances 0.000 claims description 9
- 229920002545 silicone oil Polymers 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 235000019271 petrolatum Nutrition 0.000 claims description 3
- 150000005846 sugar alcohols Polymers 0.000 claims description 3
- 229940088598 enzyme Drugs 0.000 description 76
- -1 polysiloxane Polymers 0.000 description 24
- 238000009472 formulation Methods 0.000 description 21
- 229920001296 polysiloxane Polymers 0.000 description 14
- 239000000463 material Substances 0.000 description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 10
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 9
- 239000002518 antifoaming agent Substances 0.000 description 9
- 229910019142 PO4 Inorganic materials 0.000 description 8
- 108091005804 Peptidases Proteins 0.000 description 8
- 239000004365 Protease Substances 0.000 description 8
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 8
- 108010003855 mesentericopeptidase Proteins 0.000 description 8
- 235000021317 phosphate Nutrition 0.000 description 8
- 235000019832 sodium triphosphate Nutrition 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 239000000725 suspension Substances 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 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 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 229920004482 WACKER® Polymers 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000010452 phosphate Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- TTZMPOZCBFTTPR-UHFFFAOYSA-N O=P1OCO1 Chemical class O=P1OCO1 TTZMPOZCBFTTPR-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 4
- 239000003945 anionic surfactant Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- 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 4
- 239000003381 stabilizer Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005187 foaming Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000002304 perfume Substances 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 3
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 229940048842 sodium xylenesulfonate Drugs 0.000 description 3
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 3
- 235000013162 Cocos nucifera Nutrition 0.000 description 2
- 244000060011 Cocos nucifera Species 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 108010049190 N,N-dimethylcasein Proteins 0.000 description 2
- 239000004111 Potassium silicate Substances 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 108010056079 Subtilisins Proteins 0.000 description 2
- 102000005158 Subtilisins Human genes 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 150000004996 alkyl benzenes Chemical class 0.000 description 2
- 150000008051 alkyl sulfates Chemical class 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 2
- 235000011180 diphosphates Nutrition 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 239000012669 liquid formulation Substances 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 108010020132 microbial serine proteinases Proteins 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 2
- 229910052913 potassium silicate Inorganic materials 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000001509 sodium citrate 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
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 159000000000 sodium salts Chemical class 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
- 239000002689 soil Substances 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical class OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 description 1
- FKKAGFLIPSSCHT-UHFFFAOYSA-N 1-dodecoxydodecane;sulfuric acid Chemical compound OS(O)(=O)=O.CCCCCCCCCCCCOCCCCCCCCCCCC FKKAGFLIPSSCHT-UHFFFAOYSA-N 0.000 description 1
- KYARBIJYVGJZLB-UHFFFAOYSA-N 7-amino-4-hydroxy-2-naphthalenesulfonic acid Chemical compound OC1=CC(S(O)(=O)=O)=CC2=CC(N)=CC=C21 KYARBIJYVGJZLB-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229910002016 Aerosil® 200 Inorganic materials 0.000 description 1
- 239000004382 Amylase Substances 0.000 description 1
- 108010065511 Amylases Proteins 0.000 description 1
- 102000013142 Amylases Human genes 0.000 description 1
- HSOLPAFROQCEQW-UHFFFAOYSA-N Antibiotic SEK 15 Natural products Cc1cc(O)cc(O)c1C(=O)c2c(O)cc(O)cc2CC3=CC(=O)C=C(O)O3 HSOLPAFROQCEQW-UHFFFAOYSA-N 0.000 description 1
- KPOSMBIRQBXNPA-UHFFFAOYSA-J C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C=C.[Na+].[Na+].[Na+].[Na+] Chemical compound C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C=C.[Na+].[Na+].[Na+].[Na+] KPOSMBIRQBXNPA-UHFFFAOYSA-J 0.000 description 1
- 229910021532 Calcite Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 108090000489 Carboxy-Lyases Proteins 0.000 description 1
- 102000004031 Carboxy-Lyases Human genes 0.000 description 1
- 108010059892 Cellulase Proteins 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 102000004882 Lipase Human genes 0.000 description 1
- 108090001060 Lipase Proteins 0.000 description 1
- 239000004367 Lipase Substances 0.000 description 1
- 235000008098 Oxalis acetosella Nutrition 0.000 description 1
- 240000007930 Oxalis acetosella Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 239000004280 Sodium formate Substances 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- QILXPCHTWXAUHE-UHFFFAOYSA-N [Na].NCCN Chemical compound [Na].NCCN QILXPCHTWXAUHE-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- VJHCJDRQFCCTHL-UHFFFAOYSA-N acetic acid 2,3,4,5,6-pentahydroxyhexanal Chemical compound CC(O)=O.OCC(O)C(O)C(O)C(O)C=O VJHCJDRQFCCTHL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 125000005529 alkyleneoxy group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 235000019418 amylase Nutrition 0.000 description 1
- 230000003042 antagnostic effect Effects 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000004851 dishwashing Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 1
- 229940043264 dodecyl sulfate Drugs 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 150000004675 formic acid derivatives Chemical class 0.000 description 1
- 125000003976 glyceryl group Chemical group [H]C([*])([H])C(O[H])([H])C(O[H])([H])[H] 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- TVHALOSDPLTTSR-UHFFFAOYSA-H hexasodium;[oxido-[oxido(phosphonatooxy)phosphoryl]oxyphosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O TVHALOSDPLTTSR-UHFFFAOYSA-H 0.000 description 1
- 239000003752 hydrotrope Substances 0.000 description 1
- 230000003165 hydrotropic effect Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- WPFVBOQKRVRMJB-UHFFFAOYSA-N hydroxycitronellal Chemical compound O=CCC(C)CCCC(C)(C)O WPFVBOQKRVRMJB-UHFFFAOYSA-N 0.000 description 1
- 150000002462 imidazolines Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- VMPHSYLJUKZBJJ-UHFFFAOYSA-N lauric acid triglyceride Natural products CCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCC)COC(=O)CCCCCCCCCCC VMPHSYLJUKZBJJ-UHFFFAOYSA-N 0.000 description 1
- 235000019421 lipase Nutrition 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 150000002641 lithium Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- KJPHTXTWFHVJIG-UHFFFAOYSA-N n-ethyl-2-[(6-methoxypyridin-3-yl)-(2-methylphenyl)sulfonylamino]-n-(pyridin-3-ylmethyl)acetamide Chemical compound C=1C=C(OC)N=CC=1N(S(=O)(=O)C=1C(=CC=CC=1)C)CC(=O)N(CC)CC1=CC=CN=C1 KJPHTXTWFHVJIG-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
- 239000003960 organic solvent Substances 0.000 description 1
- 125000005375 organosiloxane group Chemical group 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- PTMHPRAIXMAOOB-UHFFFAOYSA-N phosphoramidic acid Chemical class NP(O)(O)=O PTMHPRAIXMAOOB-UHFFFAOYSA-N 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 235000019419 proteases Nutrition 0.000 description 1
- 230000002797 proteolythic effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 229940077386 sodium benzenesulfonate Drugs 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- DZCAZXAJPZCSCU-UHFFFAOYSA-K sodium nitrilotriacetate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC([O-])=O DZCAZXAJPZCSCU-UHFFFAOYSA-K 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- KVCGISUBCHHTDD-UHFFFAOYSA-M sodium;4-methylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1 KVCGISUBCHHTDD-UHFFFAOYSA-M 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 108010075550 termamyl Proteins 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 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
- 229940099259 vaseline Drugs 0.000 description 1
- 239000004549 water soluble granule Substances 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
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38663—Stabilised liquid enzyme compositions
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
Description
i
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Den foreliggende opfindelse angår beskyttede enzym-systemer, som er egnede til opbevaring eller anvendelse i omgivelser, som er tilbøjelige til at forårsage nedbrydning af enzymer, såsom flydende detergenter til vask af tøj.
5 Enzymer anvendes almindeligvis til smudsfjernet ses midler i pulverdetergenter, men deres inkorporering i flydende vaskepræparater inklusive flydende detergenter til vask af tøj, såsom de, der er beskrevet i f.eks. GB 2 123 846 og GB 2 153 380, har indtil nu .^kabt alvorlige problemer. De 10 flydende formuleringer, som er mest effektive til smudsfjernelse, forårsager en hurtig nedbrydning af vaskeenzymer, hvor resultatet ofte er et signifikant tab af evnen til at fjerne pletter efter kun få dages opbevaring. Den relativt høje alkalinitet for de mere effektive smudsfjernelses-15 formuleringer og den kemiske virkning af de fleste systemer af "builder" (sekvestreringsmiddel) og de tilstedeværende overfladeaktive stoffer er specielt antagonistisk overfor detergentenzymer, og har for en stor del hindret anvendelsen af disse i sådanne detergenter, men en betydelig forringelse 20 kan ses selv i forholdsvis ikke-alkaliske sammensætninger, som er blevet specielt formuleret til at tillade inkorporering af enzymer. Selv i pulverdetergenter ses en vis nedbrydning af enzymer, især hvis pulveret er stærkt alkalisk som i maskin-opvaskepulver, eller indeholder oxiderende blegemiddel såsom 25 perborat.
Vi har nu opdaget, at nedbrydningen af enzymer i fjendtlige omgivelser, såsom flydende detergenter, reduceres væsentligt, når enzymerne dispergeres i et hydrofobt materiale, forudsat, at sidstnævnte er uopløseligt i de på-30 gældende omgivelser. Vi har ydermere opdaget, at det beskyttede enzym kan udføre sin normale funktion forudsat, at det hydrofobe materiale er tilstrækkeligt flydende eller løst til at blive opløst under anvendelsesbetingelserne.
DK ansøgning nr. 3234/78 omtaler ikke-støvende 35 enzymholdige partikler overtrukket med et vandskyende middel til anvendelse i vaskemidler i pulverform. DK 3234/78 omtaler
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2 imidlertid ikke anvendelse af enzym i flydende rensemidler, den omtaler ikke enzym dispergeret i en hydrofob væske, og den omtaler ikke nogen forbedring af enzymets lagerstabilitet.
Ifølge en udførelsesform tilvejebringer vor opfind-5 else derfor et beskyttet enzymsystem til opbevaring før anvendelse i omgivelser, der forårsager tiltagende nedbrydning af ubeskyttede enzymer, hvilket system hovedsageligt består af en dispersion af mindst et enzym i et hydrofobt stof, som er uopløseligt i de nævnte omgivelser, og som er tilstrækkeligt 10 flydende eller løst til at blive brudt under de normale anvendelsesbetingelser.
Ifølge et foretrukket aspekt tilvejebringer vor opfindelse et beskyttet enzymsystem til brug i en flydende rensesammensætning, hvilket system består af mindst et deter-15 gentenzym, der er dispergeret i et hydrofobt stof, som er uopløselig i det flydende detergent, men kan deri dispergeres som partikler eller smådråber, og som er tilstrækkelig flydende eller løst til at blive opbrudt under rense-betingelserne.
20 Ifølge en anden udførelsesform tilvejebringer vor opfindelse et beskyttet enzymsystem til brug i flydende detergentsammensætninger, der i det væsentlige består af en dispersion af et detergentenzym i en hydrofob væske, som er uopløselig i flydende detergent.
25 Ifølge en tredje udførelsesform tilvejebringer vor opfindelse en flydende rensesammensætning, hvori er dispergeret partikler eller små dråber af et beskyttet enzymsystem ifølge vor opfindelse som beskrevet i det foregående.
Henvisninger heri til opløselighed i et medium 30 refererer til både opløsning i en vandig eller anden kontinuert fase af opløsningsmiddel i mediet og til opløselig-gørelse i miceller af overfladeaktivt stof eller enhver anden diskontinuert fase, der er dispergeret i mediet.
Det hydrofobe materiale kan være en organisk poly-35 siloxanolie, f.eks. en polydi(alkyl)siloxan, hvor alkylgruppen fortrinsvis har fra 1 til 4 kulstofatomer, især en polydi-(methyl)siloxan. Specielt foretrukket er hydrofobe væsker, som
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3 er blevet stabiliseret ved at deri suspendere partikler af hydrobobt fast stof. Eksempler omfatter silikonesammensætningerne, som er foreslået til brug som skumdæmpningsmiddel i flydende detergenter, der består af hydrofob silikoneolie og 5 hydrofob silica, f.eks. en findelt silica med en silikone, der i det mindste er delvis bundet til overfladen af silicapar-tiklerne. Til eksempel kan en hydroxy funktionel organosiloxan være kondenseret med silicaoverfladens hydroxygrupper.
Eksempler på sådanne sammensætninger omfatter de der sælges 10 under de registerede varemærker "WACKER" Antifoam S132, "BEVALOID" 4237, "UNION CARBIDE" Y1206 eller DIAMOND SHAMROCK'S "NOPCO" 8315. Silikone skumdæmpningsmiddel kan være fortyndet med en umodificeret silikoneolie, såsom en polydi-methylsiloxan. Endvidere kan silikonens viscositet være for-15 øget ved tilsætning af findelt silica, f.eks. brændt silica såsom Degussa's AEROSIL® 200.
Subsidiært kan det hydrofobe materiale være en hydrocarbon med høj molekylvægt, f.eks. "petroleum bright stock" eller en såkaldt "petroleum jelly", en alkohol med høj 20 molekylvægt, f.eks. mere end 28 kulstofatomer eller en fluo-carbon med høj molekylvægt eller en hydrofob fosfatester såsom en mono- og/eller di- fedtalkylfosfatester eller et salt deraf, især et natrium eller calciumsalt eller et trialkyl-eller triarylfosfat. Hydrofobe flydende materialer kan yder-25 ligere være stabiliseret ved at inkludere hydrofobe faste partikler, f.eks. de, der er dannet ved kondensering af silica med silikone som ovenfor beskrevet eller med en fedtalkohol.
Ifølge en udførelsesform kan det hydrofobe materiale være et fast eller voksagtigt materiale ved stuetemperatur, som har et 30 blødgørings- eller fortrinsvis smeltepunkt under normal vasketemperatur, f.eks. under 60°C, fortrinsvis under 50°C, mere almindeligt 40°C, ofte under 30°C. Sådanne faste materialer tilvejebringer produkter, som er specielt egnede til anvendelse i pulver- så vel som flydende detergenter. Typisk fore-35 træklker vi, at vort hydrofobe materiale har en viskositet større end 0,05 Pascalsekunder ved normal opbevaringstemperatur (f.eks. stuetemperatur) fortrinsvis større end 0,2, mere
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4 fortrinsvis større end 0,5, og mest fortrinsvis større end 0,8 Pascalsekunder. Specielt foretrækker vi, at viskositeten skal være større end 1,0, f.eks. større end 2 og specielt større end 10 Pascalsekunder. Vi foretrækker, at viskositeten skal 5 være mindre end 200 Pascalsekunder, mest fortrinsvis mindre end 100 Pascalsekunder, f.eks. mindre end 60 Pascalsekunder og specielt mindre end 40 Pascalsekunder ved temperaturen for anvendelse. Flydende materialer, der har en viskositet mellem 1 og 50 Pascalsekunder ved stuetemperatur er specielt egnede.
10 Medmindre det modsatte er angivet er alle henvis ninger heri til viskositeter som målt ved en forskydnings-gradient på 24 see ^ og ved 25°C.
Enzymet kan f.eks. være et detergentenzym, såsom en protease, lipase, amylase, decarboxylase eller cellulase, 15 såsom de, der sælges af Novo Industri A/S under de registrerede varemærker "SAVINASE", "TEKMAMYL", "ESPERASE" og "ALCALASE" eller andre enzymer, som er aktive ved fjernelsen eller udbedringen af smuds eller pletter, eller en blanding af sådanne enzymer.
20 Enzymet kan være tilstede i det hydrofobe materiale i form af dispergerede små dråber af en enzymopløsning, f.eks. i vand eller en lavere, fortrinsvis vandblandbar mono-, dieller polyvalent alkohol, såsom propylenglycol og som kan indeholde et enzymstabiliseringsmiddel således som i den 25 kendte teknik. Enzymstabiliseringsmidler som kan være tilstede indbefatter lavere alkoholer, f.eks. glycerol, lavere monoeller di-carbonsyrer og deres salte, især formiater og oxa-later, borater og kalciumsalte.
Som et alternativ kan enzymet være tilstede i form 30 af suspenderede partikler af et fast stof indeholdende enzymer, hvor det faste enzym fortrinsvis er fremkommet ved tørring eller fældning fra en enzymopløsning, der om ønsket kan indeholde et stabiliseringsmiddel som ovennævnt, f.eks. som beskrevet i US 3,723,250, især i spalte 12; EP 0 006 638, 35 eksempel 2a og b; GB 1 296 839; US 4,435,307; EP 0 130 064 eller belgisk patentskrift 889336.
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Enzymet kan også være tilstede i et vandopløseligt granulat eller marume. Typisk sælges enzymer i denne form kommercielt. Et opløseligt krystallinsk kulhydrat såsom sucrose eller et salt såsom natriumklorid, natriumkarbonat 5 eller natriumsulfat kan således være granuleret eller marume-riseret med enzymet, og efter eget valg med enzymstabiliseringsmidler, f.eks. som beskrevet i US 4,106,991 eller GB 1 362 365, side 9 og produktet dispergeret i silikone eller hydrocarbon, såsom petroleum jelly.
10 Enzymet kan inkorporeres i den inerte olie ved dispergering ved simpel omrøring. Hvor det hydrofobe materiale er fast ved stuetempratur må det først smeltes før disperge-ringen af enzymet, og derefter afkøles til stuetemperatur. Om ønsket kan dispersionen sprayafkøles for at tilvejebringe et 15 partikelformet produkt.
Enzymindholdet i det beskyttede enzymsystem kan bestemmes af den ønskede viskositet for systemet, hvor det er ønskværdigt at behandle eller lagre sidstnævnte som en væske.
Højere indhold er tilbøjelig til at tilvejebringe høje visko-20 siteter, men er mindre tilbøjelig til dannelse af sediment af det dispergerede enzym. Vi udelukker dog ikke brugen af sedimenterende systemer, forudsat at enzymerne let kan gen-dispergeres ved omrøring før systemet tilsættes til detergentsammensætningen .
25 Fortrinsvis vælges partikelstørrelsen og enzymind holdet, så der tilvejebringes en total viskositet for det beskyttede system, der er større end 0,1 Pascalsekunder, typisk større end 0,5 Pascalsekunder, specielt større end 1 Pascalsekund, mere fortrinsvis større end 2 Pascalsekunder og 30 mest fortrinsvis større end 3 og om ønsket større end 10,0 Pascalsekunder ved opbevaringsbetingelserne og mindre end 200 Pascalsekunder, mere fortrinsvis mindre end 100 Pascalsekunder, f.eks. mindre end 70 Pascalsekunder ved anvendelsesbetingelserne. Systemer, der har en viskositet i området fra 2 35 til 60 Pascalsekunder ved stuetemperatur er almindeligvis foretrukne.
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6 I de tilfælde, hvor enzym inkorporeres i systemet som en opløsning, indeholder opløsningen fortrinsvis 1 til 90 vægt-% enzymkoncentrat, f.eks. 2 til 80%, typisk 5 til 60% og dets dispersion i olien indeholder typisk 1-80, mere sædvan-5 ligt 5-70, fortrinsvis 10-60, mere fortrinsvis 15-50, f.eks.
20-40 eller 30-50 vægt-% af enzymopløsning, hvor procentsatsen er udtrykt i forhold til vægten af det totale beskyttede enzymsystem. Suspensionen af fast enzymkoncentrat i det hydrofobe materiale indeholder typisk 1 til 90, mere sædvanligt 5 10 til 80, fortrinsvis 20-60, f.eks. 30-50 eller 20-30 vægt-% af fast stof baseret på suspensionens totale vægt.
Indholdet af enzym i det beskyttede enzymsystem kan afhænge af, om det hydrofobe stof er nødvendigt for at udøve en nyttig selvstændig funktion, f.eks. som skumdæmpnings-15 middel. I de tilfælde hvor en lavtskummende sammensætning kræves kan enzymet og skumdæmpningsmidlet passende være i det samme relative forhold som de, der er nødvendige i den endelige sammensætning. Som et alternativ kan en mere koncentreret suspension af enzym fremstilles og fortyndes med mere skum-20 dæmpningsmiddel før anvendelsen, eller tilsættes til sammensætningen på samme tid eller separat fra det ekstra skumdæmpningsmiddel .
I de tilfælde hvor det hydrofobe materiale ikke er nødvendigt for at udøve nogen anden nyttig funktion end at 25 beskytte enzymet, kan enzymkoncentratet være den maximale, der er forligelig med et håndterligt produkt.
Partikelstørrelsen for det dispergerede enzym i det beskyttede enzymsystem kan variere indenfor vide grænser.
Typisk kan det dispergerede enzym have en partikelstørrelse i 30 området 1μ til 2mm, fortrinsvis 5μ til lmm, f.eks. 10μ-700μ. Enzymkoncentrater i fast form er tilbøjelige til at ligge i den lave ende indenfor ovennævnte område, flydende opløsninger dispergeres normalt med en partikelstørrelse i midten af området, f.eks. 100μ-800μ. Granulerede enzymer har sædvanlig-35 vis en partikelstørrelse, der ligger i den øverste del af området, f.eks. 300μ-1πϋη.
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Det beskyttede enzymsystem dispergeres almindeligvis uden besvær i det flydende detergent ved simpel omrøring.
Systemet kan dispergeres som partikler eller små dråber med en diameter fra 2μ til 2,5mm, mere almindeligt 5μ-500μ, fortrins-5 vis 10μ-100μ, hvor en dispergeret opløsning eller enzymkoncentrat anvendes som det beskyttede system. I de tilfælde, hvor enzymet er tilstede som et granulat er den foretrukne partikelstørrelse for systemet i det flydende detergent 500μ til lmm.
10 Dispergerings- og emulgeringsmidler kan anvendes om ønsket, men er sædvanligvis ikke foretrukne.
Fortrinsvis tilsættes sammensætningerne til et flydende detergent, som består af en vandig fase, overfladeaktivt stof, tilstrækkelig elektrolyt opløst i den vandige 15 fase til sammen med det overfladeaktive stof at danne en struktur, der er i stand til at støtte opslemmede partikler, og et beskyttet enzymsystem ifølge vor opfindelse, der er opslemmet i detergentsammensætningen.
Fortrinsvis indeholder sammensætningen en effektiv 20 mængde detergent-"builder". Egnede "builders" omfatter kondenserede fosfater, især natriumtripolyfosfat eller, mindre fortrinsvis kaliumpyrofosfat eller natriumtetrafosfat, natrium-carbonat, natriumsilicat, natriumorthofosfat, natriumcitrat, natriumnitrilotriacetat, et fosfanat såsom natriumethylen-25 diamintetramethylenfosfonat, natriumacetodi-fosfonat eller natriumaminotris(methylenfosfonat), natrium-methylendiamin-tetraacetat eller en zeolit. Andre mindre foretrukne "buildere" består af kalium eller lithiumanaloger af de ovenfor nævnte natriumsalte.
30 Indholdet af "builder" er typisk fra ca. 5% til ca.
40 vægt-% af den flydende detergentsammensætning, sædvanligvis 10% til 35%, fortrinsvis 15-30%, mere fortrinsvis 18% til 28%, mest fortrinsvis 20 til 27%. Blandinger af to eller flere "buildere" anvendes ofte, f.eks. natriumtripolyfosfat med 35 natriumsilicat og/eller natriumcarbonat eller med zeolit; eller natriumnitrilotriacetat med natriumcitrat.
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Fortrinsvis er "builderen" i det mindste delvis tilstede som partikler i fast form, der er suspenderet i sammensætningen .
Specielt foretrukket er flydende detergentsammensæt-5 ninger i henhold til førnævnte GB 2 123 846 eller GB 2 153 380.
Opfindelsen er også anvendelig til fremstillingen af rensesammensætninger uden builder eller sammensætninger i hvilke al "builder" er tilstede i opløsning.
10 Det overfladeaktive stof kan være et anionisk-, ikke-ionisk, kationisk, amphotert, zwitterionisk og/eller semipolart overfladeaktivt stof, som typisk kan være tilstede i koncentrationer af fra 2 til 35 vægt-% af sammensætningen, fortrinsvis 5 til 30%, mere sædvanligt 7 til 25%, f.eks. 10 15 til 20%.
Sammensætningen indeholder sædvanligvis et alkyl-benzensulfonat sammen med et eller flere overfladeaktive stoffer såsom et alkylpolyoxyalkylensulfat og/eller et ikke-ionisk overfladeaktivt stof. Sidstnævnte kan typisk være et 20 alkanolamid eller en polyoxyalkyleret alkohol.
Andre anioniske overfladeaktive stoffer omfatter alkylsulfat, alkansulfonater, olefinsulfonat, fedtsyreester, sulfonater, sæber, alkylsulfosuccinater, alkylsulfo-succinamater, taurider, isothionater og polyoxyalkylen-25 derivater af de tidligere nævnte kategorier af anionisk overfladeaktivt stof. I hvert tilfælde har det overfladeaktive stof til brug heri en alkylgruppe med et gennemsnit på fra 8 til 22, fortrinsvis 10 til 20, f.eks. 12 til 18 kulstofatomer. Alkylgrupper er fortrinsvis primære og ligekædede, men vi 30 udelukker dog ikke forgrenede eller sekundære alkylgrupper.
Når der er tale om alkoholbaserede ikke-ioniske midler foretrækkes undertiden forgrenede kæder.
Det overfladeaktive middel kan være helt eller overvejende ikke-ionisk, f.eks. en polyoxyalkyleret alkohol alene 35 eller i blanding med en polyoxyalkylenglycol. Andre ikke-
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9 ioniske overfladeaktive stoffer, som kan anvendes, omfatter polyoxyalkylerede derivater af carboxylsyre, glycerol, sorbitan, alkylphenoler, alkylolamider eller aminoxider.
Alle henvisninger heri til polyoxyalkylengrupper er 5 fortrinsvis til polyoxyethylengrupper, eller mindre fortrinsvis til polyoxypropylen eller blandet oxyethylen, oxypropy-lenkopolymere eller block kopolymere grupper eller til sådanne grupper med en eller flere glycerylgrupper. Fortrinsvis har polyoxyalkylengrupperne fra 1 til 30, mere sædvanligt 2 til 10 20, f.eks. 5 til 15 alkylenoxyenheder.
Kationiske overfladeaktive stoffer til brug ifølge vor opfindelse består af kvaterniserede alkylaminer, amido-aminer og imidazoliner. Amfoteriske overfladeaktive stoffer består af betainer og sulfobetainer.
15 I almindelighed kan ethvert overfladeaktivt stof, der er refereret til i GB 1 123 846 eller i "Surface Active Agents and Detergent" af Schwartz, Perry og Berch, anvendes.
pH for den flydende detergentsammensætning er fortrinsvis alkalisk, f.eks. ca. 7,5, især 7,5 til 12 typisk 8 20 til 11, f.eks. 9 til 10,5.
Fortrinsvis indeholder den flydende detergentsammensætning opløst elektrolyt. Denne kan omfatte en opløst del af "builderen" og/eller ethvert andet salt, uorganisk eller organisk, som ikke selv er et overfladeaktivt stof, og som 25 udsalter det tilstedeværende overfladeaktive stof fra opløsningen (inklusive micellær opløsning). Eksempler omfatter natriumklorid, natriumnitrat, natriumbromid, natriumiodid, natriumborat, natriumformiat eller natriumacetat eller tilsvarende kaliumsalte. Elekrolyten er dog fortrinsvis et salt, 30 som er nødvendigt for at udøve en nyttig funktion i vaske-flotten.
Elektrolyten kan omfatte natriumsulfat i mindre koncentrationer, men elektrolytblandinger, der indeholder koncentrationer af natriumsulfat på ca. 3% eller derover, 35 baseret på detergentsammensætningens totale vægt, anvendes fortrinsvis ikke, fordi de fremkalder uønsket krystallisering ved henstand.
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Detergentsammensætningen kan indeholde enhver af de sædvanlige mindre betydelige ingredienser såsom smudssuspensionsmidler (f.eks. carboxymethylcellulose), optisk hvidt, parfume, farvestof og om ønsket et blegemiddel.
5 Særligt foretrukne flydende detergenter er de, der indeholder langkædede, f.eks. lineær- alkylbenzen- sulfonater i en mængde på 5-12%, langkædede alkylætersulfater, f.eks. med 1-5 ethyleneoxyenheder i en mængde på 0-3%, fedt-syrealkanolamider, f.eks. diethanolamider i en mængde på 1-5%, 10 blandinger af mono og di langkædede alkylfosfater i en mængde på 0-3%, f.eks. 0,1-1%, natriumtripolyfosfat (fortrinsvis før-hydratiseret med fra 0,5 til 5 vægt-% af vand) i en mængde på 14-30%, f.eks. 14-18% eller 20-30% og om ønsket natrium-carbonat i en mængde på op til 10%, f.eks. 5-10% med totalen 15 af natriumtripolyfosfat og carbonat på 20-30%, antiredeposi-tion-midler såsom natriumcarboxymethylcellulose i mængde på 0,05-0,5%, optisk hvidt i mængde på 0,05-0,5%, chelerings-midler, f.eks. aminofosfonater såsom methylenfosfonater af di-og polyaminer, især natriumethylendiamintetra(methylen-20 fosfonat) eller diethylentriaminhexa(methylenfosfonat), der om ønsket er tilstede i mængde på 0,1-1% sammmen med konventionelle additiver såsom parfume, og hvor resten er vand, hvor procentsatserne er i forhold til vægten af det totale flydende detergent. Det flydende detergent kan have en pH på 6 til 13, 25 fortrinsvis 7 til 12, sædvanligvis 8 til 11, f.eks. 9 til 10,5.
Sammensætningerne i henhold til opfindelsen kan typisk indeholde 0,01 til 10%, f.eks. 0,05-0,5 vægt-% af det beskyttede enzymsystem.
30 Flydende opvaskesammensætninger ifølge vor op findelse består typisk af letopløselige "builders" såsom kaliumpyrofosfat og/eller kaliumsilicat i en total koncentration af 10 til 30 vægt-%, overfladeaktive stoffer, fortrinsvis ikke-ioniske i koncentrationer på 0,2 til 5 vægt-% og hydro-35 troper såsom natriumxylensulfonat, natriumtoluensulfonat eller natriumbenzensulfonat i koncentrationer på 1 til 10 vægt-%.
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Rensemidler til hårde overflader ifølge vor opfindelse kan typisk bestå af 1 til 10% overfladeaktivt stof, typisk ikke-ionisk eller anioniske/ikke-ioniske blandinger, 1 til 10% hydrotrop og 2 til 20% opløselig "builder" såsom 5 kalium-pyrofosfat. Rensemidler til hårde overflader kan også, om ønsket, indeholde slibemidler såsom silica eller calcium-carbonat som arragonit eller calcit, der er opslemmet i en struktureret væske.
Tæpperensemidler ifølge vor opfindelse kan ifølge 10 vor opfindelse omfatte relativt høje koncentrationer, f.eks. 5 til 20 vægt-%, af højtskummende overfladeaktive stoffer såsom blandinger af anioniske overfladeaktive stoffer (f.eks. alkyl-sulfat) med skummemidler (f.eks. alkanolamider).
Rensemidler til ovne ifølge vor opfindelse kan være 15 af kaustiktype indeholdende f.eks. 4 til 12% alkalier såsom natriumhydroxid, og typisk et højtskummende anionisk overfladeaktivt stof såsom natriumalkylætersulfat, ellers af typen baseret på opløsningsmiddel indeholdende f.eks. 10 til 30% vandblandbare organiske opløsningsmidler såsom en lavere mono-20 di- eller polyvalent alkohol eller anden alkohol, f.eks.
propylenglycol og typisk et ikke-ionisk overfladeaktivt stof, fortrinsvis sammen med en "builder" såsom natriumtripoly-fosfat.
Eventuelle vanskeligheder ved at dispergere det 25 beskyttede enzymsystem i enhver af de foregående flydende formuleringer undgås almindeligvis ved tilsætning af små mængder konventionelle dispergeringsmidler eller opløsningsmidler såsom opløselige gummiarter eller polyelektrolyter.
De normale vaskebetingelser for detergenter til vask 30 af tøj indebærer temperaturer på fra 50°C til 60°C og en vaskeflotte indeholdende ca. 2 til 15 gm pr. liter detergent-sammensætning under kraftig omrøring. Nogle detergenter er dog formuleret og anbefales til brug ved kolde eller middel vasketemperaturer (henholdsvis 20 til 30, eller 30 til 40°C) enten 35 til sarte stoffer eller a.h.t. energibesparelse.
Opfindelsen illustreres med de følgende eksempler:
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Eksempel 1 12
En proteaseopløsning, solgt under det registrerede varemærke "Esperase" 8.0 L blev dispergeret i en blanding af lige vægtdele af en skumdæmpende silikoneolie, der har en 5 viskositet på 22,57 Pascalsekunder ved 24 see 1 og 25°C, som indeholder en hydroxyl-termineret polysiloxan, der er kondenseret med brændt silica i fast form, og som sælges under det registrerede varemærke "Wacker" Antifoam S132, og en neutral polysiloxanolie, der sælges under det registrerede varemærke 10 "Wacker" AK50. Silikoneblandingen havde en viskositet på 3,4 Pascalsekunder. Den fremstillede dispersion indeholdt 38 vægt-% af enzymopløsningen, baseret på den totale vægt af dispersionen, og havde en viskositet på 11,9 Pascalsekunder ved 24 see ^ og 25°C.
15 Dispersionen inkorporeredes med grundig omrøring i et flydende builderholdigt detergent, hvilket gav følgende formulering: vægt%
Natrium lineær alkylbenzensulfonat 9,3 20 Natrium lineær C^-IS alkylætersulfat indeholdende et gennemsnit på 3 ethylenoxyenheder pr. molekyle 1,85
Kokosnød diethanolamid 1,85
Natriumtripolyfosfat 16,7
Natriumcarbonat 6,7 25 Natriumcarboxymethylcellulose 0,9
Optisk hvidt 0,1
Enzymdispersion 3 pH 10,5-11,0
Vand resten 30 Denne formulering blev sammenlignet med den samme formulering uden enzym som kontrol ved smudsfjernelse fra en prøve af bomuld besmudset med blod, mælk og kul (EMPA 116) i en koncentration på 5gl ^ i vaskevand indeholdende 200 ppm kalciumcarbonat ved en vasketemperatur på 60°C i 30 minutter.
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13 Følgende procentdele for smudsfjernelse blev iagttaget:
Kontrol 36%
Friskfremstillet formulering 57%
Formulering efter henstand i 22 dage ved 30°C 52% 5 Eksempel 2 og 3
En 25 vægt-% suspension blev fremstillet ved at omrøre "ESPERASE®" proteasekoncentrat i fast form (fremstillet som beskrevet i U.S. patentskrift nr. 3,723,250 i spalte 12) i en silikoneolie med en viskositet på 1,83 Pascalsekunder, som 10 blev solgt af Diamond-Shamrock under varemærket "NOPCO 8315" silikone defoamer.
Opløsningen havde en viskositet på 7,32 Pascalsekunder og blev inkorporeret i builderholdige flydende detergenter, hvilket gav følgende formulering: 15 Eks. 2 Eks. 3
Natriumdodecylbenzensulfonat 6 % 7 %
Natrium lineær C]_2-18 alkylætersulfat indeholdende et gennemsnit på 3 ethylenoxyenheder pr. molekyle 2% 20 Kokosnød diethanolamid 1,5 % 3 %
Blandinger af mono og di c^g_2_g alkylfosfatester 0,5 % 0,5 %
Natriumtripolyfosfat 24 % 24 %
Natriumcarboxymethylcellulose 0,1% 0,1% 25 Enzymsuspension i silikoneolie 1,25% 1,25%
Optisk hvidt 0,2% 0,2%
Diethylentriaminpenta(methylen- fosfonat)natriumsalt 0,5 % 0,5 %
Parfume 0,3 % 0,3 % 30 Vand til 100% til 100% pH ca 9,0 ca 9,0
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14
Proteaseaktiviteten af formuleringen i eksempel 2 var 15,4 kilo Novo proteaseenheder (kilo Novo protease units = KNPU) per g.
Eksempel 4 og 5 5 På samme måde som i eksempel 2 og 3 blev en 25 vægt-% suspension af "ESPERASE®" proteasekoncentrat i fast form i en anden silikone skumdæmpningsolie, der havde en viskositet på 1,22 Pascalsekunder ("BEVALOID®" 4237), fremstillet og inkorporeret i den flydende builderholdige 10 formulering som i eksempel 2 og 3 for at give den tilsvarende formulering for henholdsvis eksempel 4 og 5. Suspensionen havde en viskositet på 3,66 Pascalsekunder.
Proteaseaktiviteten for formuleringen i eksempel 4 var 14,8 KNPU per g.
15 Lagerstabilitetundersøgelse
Stabiliteten for formuleringerne i eksempel 2 og 4 ved opbevaring ved 37°C i 5 uger blev bestemt og sammenlignet med den tilsvarende sammenligningsformulering i eksempel 2 med den samme mængde enzym men ingen silikoneolie.
20 Den proteolytiske restaktivitet for hver formulering blev bestemt ved dimethylcasein (DMC) metoden beskrevet i Novo publikation AF 101/4-GB. Resultaterne vises i nedenstående tabel med aktivitet udtrykt som procentdel af den initiale aktivitet for den pågældende formulering.
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15 _Restaktiviteten efter tid i uger
Formulering_2_4_5_
Eksempel 2 80% 70% 70%
Eksempel 4 85% 65% 63% 5 Sammmenligning_33%_9%_i.a._ (i.a. = ikke analyseret)
Eksempel 6 til 13
Et antal alternative beskyttede enzymsystemer blev hver især fremstillet ved at omrøre 25% enzymkoncentrat i fast 10 form i hydrofoben og blev testet som vist i nedenstående tabel: I I Varemærke | Kemisk | Viskositeten [Viskositeten
Eks. I I for I type af j P.sek af j af system nr. j Enzym | hydrofob j hydrofob j hydrofob j i P.sek 15 I i I Silikoneolie +1 ] 6 I "TERMAM¥L®" | "BEVALOID®" jhydrofob j 1,22 j 2,44 I_ ί_1 silica___ ~7 I "SAVINASE®" | | :Γ_ΪΓ^ | - | 2/74 I "ALCALASE®" | | 2713 20 [ I "WACKER®" I Silikoneolie +| [ 9 I - " - I S132 + (hydrofob | | 9,76 I I "WACKER®” I silica for- | j I I AK50 I tyndet m. oliej j
To I "TERMAMYL^ - " - [ - " - | | 10,06 25 I i "CATANEX®" [Petroleum | | 11 I "ESPERASE®" [ 79_bright stock 1,62 4,09 [ I [Petroleum | [ 12 I "ESPERASE®" | "VASELINE®" | jelly___ I 1 [bl. mono/di [ [ 30 13 I"ESPERASE®"I "EMPICOL®" Ι^16_18 alkyl- | | I I 7062P I surt fosfat | | 1 I I Silikoneolie + | | 13A I"ESPERASE®"i "WACKER®" |hydrofob | 22,7 | _j_I S132_I silica_j_\_ 35 Alle eksemplerne 6 til 13A blev anvendt som enzymsystemet i en prøve af et flydende detergent i henhold til eksempel 3. De viste sig alle at udvise væsentlig
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16 forbedret evne til at bibeholde enzymaktiviteten og smudsfjernelsen sammenlignet med ubeskyttede enzymer ved opbevaring i to uger ved stuetemperatur.
Eksempel 14 5 Et flydende opvaskemiddel har følgende formulering: 30% aktivt vandigt natriumxylensulfonat ("ELTESOL®" SX30) 10% 80% aktiv vandig syntetisk alkohol 8 mol ethyoxylat ("EMPILAN®" KA880) 0,5% 10 Kaliumhydroxid 1%
Tetrakaliumpyrofosfat 15%
Kaliumsilicat 10%
Eksempel 9 0,5%
Vand balance 15 Eksempel 15
Et rensemiddel til hårde overflader har følgende formulering: 30% natriumxylensulfonat ("ELTESOL®" SX30) 10% 80% syntetisk alkohol 8 mol ethoxylat 20 ("EMPILAN®" KA880) 2% 30% natriumlaurylsulfat ("EMPILAN 0" SL30) 5%
Tetrakaliumpyrofosfat 5%
Eksempel 12 0,5% 25 Vand balance
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Eksempel 16 17
Et tæpperensemiddel har følgende formulering: 14% natriumlaurylsulfat + ) 14% laurinmonoethanolamidsulfosuccinat ) 25,0% 5 ("EMPIMIN®" 3119) )
Eksempel 8 0,5%
Vand balance
Eksempel 17
Et tæpperensemiddel har følgende formulering: 10 28% natrium syntetisk laurylsulfat ("EMPICOL®" LX 288/5) 36%
Laurinisopropanolamid 2%
Eksempel 13 0,5%
Vand balance 15 Eksempel 18
Et rensemiddel til ovn har følgende formulering:
Nonylphenyl 9 mol ethoxylat ("EMPILAN®" NP9) 15%
Propylenglycol 20% 20 Natriumtripolyfosfat 10%
Eksempel 7 0,5%
Vand balance
Eksempel 19
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18
Et rensemiddel til ovn har følgende formulering: 27% laurylætersulfat ("EMPIMIN®" 27/T 20% 5 Natriumhydroxid (i fast form) 8%
Eksempel 12 0,5%
Vand balance
Claims (15)
1. Et beskyttet enzymsystem til anvendelse i flydende rensemidler, kendetegnet ved, at det består hovedsageligt af en hydrofob væske, som hovedsagelig er uopløselig i vandige 5 flydende detergenter til vask af tøj og et detergentenzym, der er dispergeret i nævnte væske.
2. Et system ifølge krav 1, kendetegnet ved, at nævnte væske har en viskositet større end 0,05 Pascalsekunder ved 25°C og en viskositet mindre end 200 Pascalsekunder ved 60°C.
3. Et system ifølge krav 2, kendetegnet ved, at nævnte væske har en viskositet større end 0,8 Pascalsekunder ved 25°C og en viskositet mindre end 100 Pascalsekunder ved 60°C.
4. Et system ifølge kravene 1-3, kendetegnet ved, at nævnte væske hovedsagelig består af en silikoneolie.
5. Et system ifølge krav 4, kendetegnet ved, at nævnte olie endvidere indeholder hydrofob silica.
6. Et system ifølge kravene 1-3, kendetegnet ved, at nævnte væske er en hydrocarbon.
7. Et system ifølge krav 6, kendetegnet ved, at nævnte væske 20 er petroleum jelly. DK 160886 B
8. Et system ifølge kravene 1 - 7, kendetegnet ved, at nævnte hydrofobe væske indeholder dispergerede små dråber af en opløsning af nævnte enzym i et opløsningsmiddel, der er udvalgt fra gruppen bestående af vand og vandblandbare mono- 5 di- og polyvalente alkoholer.
9. Et system ifølge kravene 1-7, kendetegnet ved, at nævnte hydrofobe væske indeholder dispergerede partikler af et enzymkoncentrat i fast form.
10. Et system ifølge kravene 1-9, kendetegnet ved, at 10 partikelstørrelsen af nævnte dispergerede enzym er fra 5μ til 1 mm.
11. En flydende rensemiddelsammensætning, kendetegnet ved, at den består hovedsagelig af vand, overfladeaktivt stof og et dispergeret detergentenzym ifølge krav 1.
12. En rensemiddelsammensætning ifølge krav 11 bestående hovedsagelig af vand, overfladeaktivt stof og et dispergeret enzymsystem, hvilket enzymsystem hovedsagelig består af nævnte hydrofobe væske, hvori nævnte enzym er dispergeret.
13. En rensemiddelsammensætning ifølge kravene 11 - 12, 20 kendetegnet ved, at det består hovedsagelig af fra 5 til 30% overfladeaktivt stof, fra 5 til 40% "builder” og deri dispergeret et indhold af af nævnte enzymsystem.
14. En rensemiddelsammensætning ifølge kravene 11 - 13, kendetegnet ved, at nævnte beskyttede enzymsystem har en 25 partikelstørrelse på fra 2μ til 2,5 mm.
15. En rensemiddelsammensætning ifølge krav 11, kendetegnet ved, at detergentenzymet er dispergeret i en hydrofob væske, der har en viskositet større end 0,05 Pascalsekunder ved 25°C og en viskositet mindre end 200 Pascalsekunder ved 60°C.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB8604164 | 1986-02-20 | ||
| GB868604164A GB8604164D0 (en) | 1986-02-20 | 1986-02-20 | Enzymatic liquid detergent compositions |
| GB8616137 | 1986-07-02 | ||
| GB868616137A GB8616137D0 (en) | 1986-07-02 | 1986-07-02 | Enzymatic liquid detergent compositions |
Publications (4)
| Publication Number | Publication Date |
|---|---|
| DK86187D0 DK86187D0 (da) | 1987-02-20 |
| DK86187A DK86187A (da) | 1987-08-21 |
| DK160886B true DK160886B (da) | 1991-04-29 |
| DK160886C DK160886C (da) | 1991-10-21 |
Family
ID=26290373
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DK086187A DK160886C (da) | 1986-02-20 | 1987-02-20 | Et beskyttet enzymsystem og en flydende rensemiddelsammensaetning indeholdende dette |
Country Status (17)
| Country | Link |
|---|---|
| US (1) | US4906396A (da) |
| EP (1) | EP0238216B1 (da) |
| CN (1) | CN87100752A (da) |
| AU (1) | AU594120B2 (da) |
| DE (1) | DE3762629D1 (da) |
| DK (1) | DK160886C (da) |
| EG (1) | EG18543A (da) |
| ES (1) | ES2015572B3 (da) |
| FI (1) | FI870726A7 (da) |
| GB (1) | GB2186884A (da) |
| GR (1) | GR3000585T3 (da) |
| HU (1) | HUT44286A (da) |
| NO (1) | NO870679L (da) |
| NZ (1) | NZ219353A (da) |
| PL (1) | PL154945B1 (da) |
| PT (1) | PT84338B (da) |
| TR (1) | TR23421A (da) |
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Family Cites Families (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2642376A (en) * | 1949-08-12 | 1953-06-16 | Pillsbury Mills Inc | Protected enzyme preparation |
| DE1617190A1 (de) * | 1966-04-25 | 1971-02-18 | Procter & Gamble Europ | Koerniges,Enzyme enthaltendes Waschmittel |
| RO57973A (da) * | 1969-06-13 | 1975-03-15 | ||
| BE755046A (da) * | 1969-09-01 | 1971-02-01 | Salkin Nicolas | |
| IT989051B (it) * | 1971-04-23 | 1975-05-20 | Snam Progetti | Procedimento per la produzione enzimatica di l triptofano |
| BE788554A (fr) * | 1971-09-23 | 1973-01-02 | Rech Applic Scient Sogeras S A | Procede pour la fabrication de substances actives pulverisees protegeescontre un milieu biologique |
| JPS5423994B2 (da) * | 1972-03-25 | 1979-08-17 | ||
| GB1590432A (en) * | 1976-07-07 | 1981-06-03 | Novo Industri As | Process for the production of an enzyme granulate and the enzyme granuate thus produced |
| US4115292A (en) * | 1977-04-20 | 1978-09-19 | The Procter & Gamble Company | Enzyme-containing detergent articles |
| FR2430453B1 (fr) * | 1978-07-04 | 1986-04-18 | Novo Industri As | Produit proteasique a pouvoir allergisant reduit |
| FR2481942B1 (fr) * | 1980-05-12 | 1988-04-22 | Unilever Nv | Granules antimousse, leur procede de fabrication et leur utilisation dans les compositions detergentes |
| IS1740B (is) * | 1982-02-05 | 1999-12-31 | Albright & Wilson Uk Limited | Samsetning á hreinsivökva |
| DK289083A (da) * | 1983-06-23 | 1984-12-24 | Novo Industri As | Lipase, fremgangsmaade til fremstilling deraf og anvendelse deraf |
| MX167884B (es) * | 1983-12-22 | 1993-04-20 | Albright & Wilson | Composicion detergente liquida |
| GB8413802D0 (en) * | 1984-05-30 | 1984-07-04 | Procter & Gamble | Detergent with suds control |
| CA1263944A (en) * | 1984-09-12 | 1989-12-19 | Barbara H. Munk | Pre-wash compositions containing enzymes |
-
1987
- 1987-02-18 EG EG87/87A patent/EG18543A/xx active
- 1987-02-19 HU HU87653A patent/HUT44286A/hu unknown
- 1987-02-20 DK DK086187A patent/DK160886C/da active
- 1987-02-20 CN CN198787100752A patent/CN87100752A/zh active Pending
- 1987-02-20 AU AU69111/87A patent/AU594120B2/en not_active Ceased
- 1987-02-20 NO NO870679A patent/NO870679L/no unknown
- 1987-02-20 GB GB08704038A patent/GB2186884A/en not_active Withdrawn
- 1987-02-20 EP EP87301487A patent/EP0238216B1/en not_active Expired - Lifetime
- 1987-02-20 TR TR114/87A patent/TR23421A/xx unknown
- 1987-02-20 US US07/016,874 patent/US4906396A/en not_active Expired - Fee Related
- 1987-02-20 ES ES87301487T patent/ES2015572B3/es not_active Expired - Lifetime
- 1987-02-20 FI FI870726A patent/FI870726A7/fi not_active Application Discontinuation
- 1987-02-20 NZ NZ219353A patent/NZ219353A/en unknown
- 1987-02-20 PL PL1987264223A patent/PL154945B1/pl unknown
- 1987-02-20 PT PT84338A patent/PT84338B/pt not_active IP Right Cessation
- 1987-02-20 DE DE8787301487T patent/DE3762629D1/de not_active Expired - Lifetime
-
1990
- 1990-06-26 GR GR90400409T patent/GR3000585T3/el unknown
Also Published As
| Publication number | Publication date |
|---|---|
| PT84338A (en) | 1987-03-01 |
| PT84338B (pt) | 1989-09-14 |
| DK86187A (da) | 1987-08-21 |
| NZ219353A (en) | 1990-04-26 |
| US4906396A (en) | 1990-03-06 |
| AU594120B2 (en) | 1990-03-01 |
| ES2015572B3 (es) | 1990-09-01 |
| NO870679L (no) | 1987-08-21 |
| AU6911187A (en) | 1987-08-27 |
| GR3000585T3 (en) | 1991-07-31 |
| HUT44286A (en) | 1988-02-29 |
| EG18543A (en) | 1993-07-30 |
| DK86187D0 (da) | 1987-02-20 |
| EP0238216A1 (en) | 1987-09-23 |
| GB8704038D0 (en) | 1987-03-25 |
| FI870726L (fi) | 1987-08-21 |
| EP0238216B1 (en) | 1990-05-09 |
| FI870726A0 (fi) | 1987-02-20 |
| GB2186884A (en) | 1987-08-26 |
| CN87100752A (zh) | 1987-11-25 |
| TR23421A (tr) | 1989-12-29 |
| DK160886C (da) | 1991-10-21 |
| PL264223A1 (en) | 1988-03-31 |
| FI870726A7 (fi) | 1987-08-21 |
| NO870679D0 (no) | 1987-02-20 |
| PL154945B1 (en) | 1991-10-31 |
| DE3762629D1 (de) | 1990-06-13 |
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