EP0120492A2 - Composante granuleuse de détergent, à écoulement libre et procédé pour sa préparation - Google Patents
Composante granuleuse de détergent, à écoulement libre et procédé pour sa préparation Download PDFInfo
- Publication number
- EP0120492A2 EP0120492A2 EP84103320A EP84103320A EP0120492A2 EP 0120492 A2 EP0120492 A2 EP 0120492A2 EP 84103320 A EP84103320 A EP 84103320A EP 84103320 A EP84103320 A EP 84103320A EP 0120492 A2 EP0120492 A2 EP 0120492A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- weight
- spray
- water
- product according
- product
- 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.)
- Granted
Links
- 239000003599 detergent Substances 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims description 29
- 230000008569 process Effects 0.000 title claims description 15
- 238000002360 preparation method Methods 0.000 title claims 3
- 239000000203 mixture Substances 0.000 claims abstract description 35
- 238000001694 spray drying Methods 0.000 claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000007921 spray Substances 0.000 claims description 43
- 239000002245 particle Substances 0.000 claims description 36
- 239000002002 slurry Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000002736 nonionic surfactant Substances 0.000 claims description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 25
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 22
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 20
- 239000010457 zeolite Substances 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 16
- 229910021536 Zeolite Inorganic materials 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 11
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- 239000003945 anionic surfactant Substances 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 8
- 229910000503 Na-aluminosilicate Inorganic materials 0.000 claims description 7
- 239000004115 Sodium Silicate Substances 0.000 claims description 7
- 230000007062 hydrolysis Effects 0.000 claims description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 235000012217 sodium aluminium silicate Nutrition 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 239000000344 soap Substances 0.000 claims description 5
- 239000000429 sodium aluminium silicate Substances 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 230000000274 adsorptive effect Effects 0.000 claims description 4
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 239000008187 granular material Substances 0.000 abstract description 20
- 239000004094 surface-active agent Substances 0.000 abstract description 18
- 229910019142 PO4 Inorganic materials 0.000 abstract description 12
- 235000021317 phosphate Nutrition 0.000 abstract description 11
- 239000000654 additive Substances 0.000 abstract description 10
- 150000003013 phosphoric acid derivatives Chemical class 0.000 abstract description 8
- 239000000725 suspension Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 69
- 239000000047 product Substances 0.000 description 36
- -1 alkali metal salts Chemical class 0.000 description 19
- 150000001875 compounds Chemical class 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 12
- 235000014113 dietary fatty acids Nutrition 0.000 description 11
- 239000000194 fatty acid Substances 0.000 description 11
- 229930195729 fatty acid Natural products 0.000 description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 10
- 239000002253 acid Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 10
- 239000004576 sand Substances 0.000 description 10
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- 238000007792 addition Methods 0.000 description 9
- 239000007844 bleaching agent Substances 0.000 description 9
- 229940088598 enzyme Drugs 0.000 description 9
- 150000004665 fatty acids Chemical class 0.000 description 9
- 239000000428 dust Substances 0.000 description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 7
- 230000036571 hydration Effects 0.000 description 7
- 238000006703 hydration reaction Methods 0.000 description 7
- 238000012545 processing Methods 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 229920000388 Polyphosphate Polymers 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 5
- 239000006260 foam Substances 0.000 description 5
- 239000003112 inhibitor Substances 0.000 description 5
- 230000001788 irregular Effects 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 5
- 239000001205 polyphosphate Substances 0.000 description 5
- 235000011176 polyphosphates Nutrition 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- GLDOVTGHNKAZLK-UHFFFAOYSA-N n-octadecyl alcohol Natural products CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 4
- 229940055577 oleyl alcohol Drugs 0.000 description 4
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 4
- 239000003760 tallow Substances 0.000 description 4
- FRPJTGXMTIIFIT-UHFFFAOYSA-N tetraacetylethylenediamine Chemical compound CC(=O)C(N)(C(C)=O)C(N)(C(C)=O)C(C)=O FRPJTGXMTIIFIT-UHFFFAOYSA-N 0.000 description 4
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 235000010290 biphenyl Nutrition 0.000 description 3
- 239000004305 biphenyl Substances 0.000 description 3
- 125000006267 biphenyl group Chemical group 0.000 description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 3
- 150000001735 carboxylic acids Chemical class 0.000 description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 150000002191 fatty alcohols Chemical class 0.000 description 3
- 229910021485 fumed silica Inorganic materials 0.000 description 3
- 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 3
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 239000002888 zwitterionic surfactant Substances 0.000 description 3
- 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 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 2
- 102000005701 Calcium-Binding Proteins Human genes 0.000 description 2
- 108010045403 Calcium-Binding Proteins Proteins 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
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- 239000001083 [(2R,3R,4S,5R)-1,2,4,5-tetraacetyloxy-6-oxohexan-3-yl] acetate Substances 0.000 description 2
- UAOKXEHOENRFMP-ZJIFWQFVSA-N [(2r,3r,4s,5r)-2,3,4,5-tetraacetyloxy-6-oxohexyl] acetate Chemical compound CC(=O)OC[C@@H](OC(C)=O)[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](OC(C)=O)C=O UAOKXEHOENRFMP-ZJIFWQFVSA-N 0.000 description 2
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- 230000008859 change Effects 0.000 description 2
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 description 2
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- 150000004985 diamines Chemical class 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical group OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- FSBVERYRVPGNGG-UHFFFAOYSA-N dimagnesium dioxido-bis[[oxido(oxo)silyl]oxy]silane hydrate Chemical compound O.[Mg+2].[Mg+2].[O-][Si](=O)O[Si]([O-])([O-])O[Si]([O-])=O FSBVERYRVPGNGG-UHFFFAOYSA-N 0.000 description 2
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
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- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 description 2
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- JIRHAGAOHOYLNO-UHFFFAOYSA-N (3-cyclopentyloxy-4-methoxyphenyl)methanol Chemical compound COC1=CC=C(CO)C=C1OC1CCCC1 JIRHAGAOHOYLNO-UHFFFAOYSA-N 0.000 description 1
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- JBVOQKNLGSOPNZ-UHFFFAOYSA-N 2-propan-2-ylbenzenesulfonic acid Chemical compound CC(C)C1=CC=CC=C1S(O)(=O)=O JBVOQKNLGSOPNZ-UHFFFAOYSA-N 0.000 description 1
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- REZZEXDLIUJMMS-UHFFFAOYSA-M dimethyldioctadecylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC REZZEXDLIUJMMS-UHFFFAOYSA-M 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
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- 239000004664 distearyldimethylammonium chloride (DHTDMAC) Substances 0.000 description 1
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 1
- DUYCTCQXNHFCSJ-UHFFFAOYSA-N dtpmp Chemical compound OP(=O)(O)CN(CP(O)(O)=O)CCN(CP(O)(=O)O)CCN(CP(O)(O)=O)CP(O)(O)=O DUYCTCQXNHFCSJ-UHFFFAOYSA-N 0.000 description 1
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000002979 fabric softener Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical group C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 125000001046 glycoluril group Chemical group [H]C12N(*)C(=O)N(*)C1([H])N(*)C(=O)N2* 0.000 description 1
- 239000003979 granulating agent Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000010438 heat treatment Methods 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
- 238000000265 homogenisation Methods 0.000 description 1
- 150000002462 imidazolines Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 235000019421 lipase Nutrition 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000010327 methods by industry Methods 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- XJRBAMWJDBPFIM-UHFFFAOYSA-N methyl vinyl ether Chemical compound COC=C XJRBAMWJDBPFIM-UHFFFAOYSA-N 0.000 description 1
- 125000000250 methylamino group Chemical group [H]N(*)C([H])([H])[H] 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 125000004573 morpholin-4-yl group Chemical group N1(CCOCC1)* 0.000 description 1
- BXWNKGSJHAJOGX-UHFFFAOYSA-N n-hexadecyl alcohol Natural products CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 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
- 125000001117 oleyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000010915 one-step procedure Methods 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 229910052615 phyllosilicate Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920001444 polymaleic acid Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- KCXFHTAICRTXLI-UHFFFAOYSA-M propane-1-sulfonate Chemical compound CCCS([O-])(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-M 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 229940048084 pyrophosphate Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 239000011833 salt mixture Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000001932 seasonal effect Effects 0.000 description 1
- 238000005029 sieve analysis Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 229940045872 sodium percarbonate Drugs 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 235000011008 sodium phosphates Nutrition 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 235000019794 sodium silicate Nutrition 0.000 description 1
- 235000019351 sodium silicates Nutrition 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000003628 tricarboxylic acids Chemical class 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229940071104 xylenesulfonate Drugs 0.000 description 1
Images
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
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/02—Preparation in the form of powder by spray drying
-
- 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
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
- C11D17/065—High-density particulate detergent compositions
Definitions
- washing powders with a high bulk density have been known for a long time. These include, for example, agents with a high soda or silicate content, as were obtained in the past, for example, by simply mixing the individual components together or by drying aqueous mixtures on trays or heated rollers, extruding or spray crystallization. These specifically heavy powders tend to cake, usually have poor solution properties and cannot be used in modern washing machines with pre-programmed cycle times.
- nonionic surfactants can be applied subsequently to the spray-dried carrier material.
- powder such as talc, finely divided silica or calcined clay.
- a graying inhibitor in powder form for example carboxymethyl cellulose, can also be added subsequently.
- the powders thus obtained, loaded with nonionic surfactants can have a bulk density of more than 500 g / l, for example 700 g / 1, and a flowability of, for example, up to 76% of that of dry sand.
- the size of these powder particles is between 3.3 mm to 0.075 mm, in particular between 0.83 and 0.15 mm ....
- Granular detergents with a bulk density of at least 500 g / l which consist of essentially spherical particles of a certain grain size and have a fluidity of 70%, based on dry sand, are known from German Offenlegungsschrift 27 42 683.
- These agents filled in a plastic bottle have a content of 30 to 80% of builders, 2 to 40% of surfactants, which are essentially non-ionic, 0 to 20% of other additives, 0 to 50% of fillers and 3 to 15% Moisture. It is true that the manufacture of the products described in this way is called arbitrary, for example also by spray drying or granulation. However, the only specifically specified and thus usable route is via a two-stage and therefore complex manufacturing process, in which one initially produces so-called "base beads" with a porous outer surface and a more or less absorbent inner frame by spray drying an aqueous slurry, which is then used the liquid or melted nonionic surfactant is sprayed or soaked.
- DE-AS 17 92 434 describes a process for the production of granular detergents with a content of 2 to 15% by weight of anionic and 5 to 20% by weight of nonionic surfactants and 25 to 60% by weight tripolyphosphate known by spray drying a slurry.
- the tripolyphosphate used to prepare the slurry must be partially prehydrated. This partial prehydration is necessary in order to produce free-flowing powders.
- the process provides loose powder with a bulk density of less than 550 g / 1 and - if the proportion of non-ionic surfactant significantly exceeds 15% by weight - only very moderate pouring properties.
- the invention by means of which the problems outlined are solved, is a granular, free-flowing, water-soluble detergent component with a bulk density of 550 to 800 g / 1, consisting of synthetic, essentially nonionic surfactants, inorganic carrier substances, other organic washing aids and adsorptive or as hydrate bound water.
- This granular detergent component is characterized in that it is produced by spray drying and is more than 50% by weight of drop-shaped to rod-shaped particles with an average diameter of 0.02 to 1.5 mm, an average length of 0.1 to 5 mm and a ratio of average diameter to average length of 1 : 1.2 to 1:10.
- This granular detergent component is the essential component of a free-flowing detergent produced by adding further powder components; however, the granular detergent component as defined above can also be the practically sole constituent of a detergent. Accordingly, the detergent component in granular form according to the invention is present in the free-flowing detergent in proportions of 15 to 100%, preferably 50 to 95%.
- Suitable alkoxylated nonionic surfactants are ethoxylated alcohols having 12 to 24, preferably 14 to 18 carbon atoms and an average of 3 to 20, preferably 4 to 16, glycol ether groups.
- the hydrocarbon residues can be saturated or monounsaturated, linear or also methyl-branched in the 2-position (oxo residue) and can be derived, for example, from naturally occurring or hydrogenated fat residues and / or synthetic residues.
- Ethoxylates derived from cetyl, stearyl and oleyl alcohol and mixtures thereof have proven to be particularly suitable.
- EO ethylene oxide groups
- tallow fatty alcohol with an average of 10 to 18 EO tallow fatty alcohol with an average of 10 to 18 EO
- oleyl alcohol with an average of 6 to 12 EO as well as their mixtures.
- Such mixtures of two and more Surfactants with different EO content, in which the proportion of higher ethoxylated alcohols predominates have proven to be particularly advantageous, since the tendency to smoke in the exhaust air (so-called pluming) is particularly low and the washing effect against mineral and fatty soiling is particularly pronounced .
- Alkoxylated alcohols have also proven to be advantageous in the sense of a low tendency to "pluming", in the production of which 1 to 3 mol of propylene oxide and then 4 to 20, preferably 4 to 7 mol, of ethylene oxide were added to the alcohol oil. You can replace components (a) and (b) in whole or in part in the aforementioned mixtures.
- non-Bibnic surfactants are those which have a similar distribution of the ethylene glycol or propylene glycol ether groups and are derived from alkylphenols, fatty amines, fatty acid amides and fatty acids.
- the ethoxylated fatty acid amides also include the fatty acid mono- or diethanolamides or the corresponding fatty acid propanolamides.
- the water-soluble ones containing 20 to 250 ethylene glycol ether groups and 10 to 100 propylene glycol ether groups can also be used Polyethylene oxide adducts with polypropylene glycol, ethylenediaminopolypropylene glycol and alkylpolypropylene 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 surfactants of the amine oxide type can also be present.
- Amine oxides containing polyglycol ether groups can also be used.
- the detergent component according to the invention contains 15 to 28% by weight, preferably 17 to 25% by weight and in particular 18 to 23% by weight, of ethoxylated nonionic surfactants.
- the content of synthetic anionic surfactants in the detergent component i.e. those of the sulfonate or sulfate type should be less than 1%, preferably less than 0.5%, in particular 0% and that of soap less than 0.2%, preferably 0%.
- No anionic surfactants are expediently used, since surprisingly it has been shown that even small amounts of such additives, in particular the smallest additions of soap, cause the granules to swell during spray drying and thus to a decrease in the desired high bulk density and free-flowing properties.
- inorganic carrier substances there are primarily builders which can also bind or precipitate the hardness constituents of the water.
- builders which includes the polymer phosphates, in particular sodium tripolyphosphate and more highly condensed polymer phosphates, such as sodium tetraphosphate.
- the polymer phosphates can be present in a mixture with their hydrolysis products, ie orthophosphate and pyrophosphate, but because of the higher washing and calcium binding capacity of the polyphophates, the lowest possible hydrolysis of the polyphosphate when preparing the slurry and during spray drying is to be aimed for by suitable measures.
- Suitable carrier substances are in particular also the synthetic bound water-containing sodium aluminosilicates of the zeolite A type. You can replace the polymer phosphates in whole or in part, i.e. their use also enables the production of phosphate-free agents.
- the zeolites are used in the usual hydrated, finely crystalline "form, ie they have practically no particles larger than 30 microns and preferably consist at least 80% of particles smaller than 10 microns.
- Their calcium binding capacity which according to According to DE 24 12 837, it is in the range of 100-200 mg CaO / g.
- Particularly useful is the zeolite NaA, also the zeolite NaX and mixtures of NaA and NaX.
- Further useful carrier substances which can be present in a mixture with the compounds mentioned above are sodium carbonate, sodium sulfate and magnesium silicate.
- Compounds with a high adsorption capacity such as finely divided silica, clays or bentonites, may also be present.
- the proportion of the inorganic carrier substance is a total of 40 to 80% by weight, based on anhydrous or non-hydrated components, preferably 45 to 70% by weight.
- the proportion of sodium tripolyphosphate (including the hydrolysis products) in the detergent component according to the invention is 0 to 60% by weight, preferably 10 to 50% by weight and in particular 20 to 40% by weight.
- the proportion of the alkali metal silicates is 5 to 20% by weight, preferably 6 to 15% by weight and in particular 6.5 to 12% by weight.
- the sodium aluminosilicate is present in proportions of 0 to 40% by weight, preferably 3 to 30% by weight and in particular 5 to 25% by weight.
- the proportion of sodium silicate can be found in such carrier salt mixtures which consist essentially of sodium tripolyphosphate or consist of zeolite and mixtures thereof, can also be increased beyond the stated maximum content of 20% by weight without resulting in major disadvantages for the dissolving behavior of the particles.
- the percentage content of polyphosphate in the detergents can be in the range of conventional heavy-duty detergents, the tendency to reduce phosphate is fully taken into account in the invention.
- the agents according to the present invention are compared to conventional, i.e. specifically light washing powders are used in a much lower dosage; on the other hand, the proportion of phosphate in favor of the proportion of aluminosilicate can be considerable, i.e. can be reduced to, for example, 10% by weight or even eliminated entirely.
- the detergent component according to the invention can additionally contain so-called co-builders as other organic washing aids, which are capable of considerably increasing the action of the polyphosphates and sodium aluminosilicates even in small amounts.
- Polyphosphonic acids or their alkali metal salts are particularly suitable as co-builders. Suitable polyphosphonic acids are 1-hydroxyethane-1,1-diphosphonic acid, aminotri- (methylene-phosphonic acid), ethylenediaminetetra- (methylenephosphonic acid) and their higher homologues, such as, for example, diethylene-triaminepenta- (methylenephosphonic acid). More co-builders are complexing aminopolycarboxylic acids.
- alkali salts of nitrilotriacetic acid and ethylenediaminotetraacetic acid include in particular alkali salts of nitrilotriacetic acid and ethylenediaminotetraacetic acid.
- the salts of diethylenetriamineopentaacetic acid and the higher homologues of the aminopolycarboxylic acid mentioned are also suitable.
- the polyacids mentioned are preferably used as sodium salts.
- co-builders are the polymeric carboxylic acids or their salts with a molecular weight of at least 350 in the form of the water-soluble sodium or potassium salts, such as polyacrylic acid, polymethacrylic acid, poly- ⁇ -hydroxyacrylic acid, polymaleic acid, polyitaconic acid, polymesaconic acid, polybutene tricarboxylic acid and the copolymers the corresponding monomeric carboxylic acids with one another or with ethylenically unsaturated compounds, such as ethylene, propylene, isobutylene, vinyl methyl ether or furan.
- the copolymer of maleic acid and acrylic acid in a ratio of 5: 1 to 1: 5 may be mentioned as an example.
- Small amounts of these co-builders are understood to mean proportions of 0.5 to 10, preferably 1 to 5,% by weight, based on the total amount of the detergent component.
- organic detergent components which may be present in the spray-dried powder component are graying inhibitors, optical brighteners and additives which regulate the viscosity behavior of the slurry, for example alkali metal salts or toluene, cumene or xylene sulfonic acid and, if appropriate, polymers which act as thickeners (for example from Carbopol type).
- Suitable graying inhibitors are, in particular, carboxymethyl cellulose, methyl cellulose, furthermore water-soluble polyesters and polyamides from polyvalent carboxylic acids and glycols or diamines, which have free carboxyl groups, betain groups or sulfobetaine groups capable of salt formation, and polymers or copolymers of vinyl alcohol, vinyl amide and acrylamide, colloidally soluble in water, acrylamides and acrylamides .
- These organic washing aid additives can be present in proportions of 0.5 to 10% by weight.
- Suitable optical brighteners are the alkali salts of 4,4-bis (-2 "-anilino-4" -morpholino-1,3,5-triazinyl-6 "- amino) -stilbene-2,2-disulfonic acid or similar compounds, which carry a diethanolamino group, a methylamino group or a .beta.-methoxyethylamino group instead of the morpholino group.
- Brighteners of the substituted diphenylstyryl type for example the alkali metal salts of 4,4-bis (2-sulfostyryl) diphenyl, 4,4-bis, are also suitable (4-chloro-3-sulfostyryl) diphenyl and 4- (4-chlorostyryl) -4- (2-sulfostyryl) diphenyl.
- the agents usually have a water content of 8 to 20% by weight, preferably 10 to 16% by weight, which means both the adsorptively bound water and the water of hydration.
- the proportion of water bound in the hydrated sodium aluminosilicate is about 20% by weight, based on the total amount of the hydrated sodium aluminosilicate; i.e. it is the degree of hydration that is in equilibrium with the environment. This proportion must be taken into account when calculating the amount of water. Basically, the water content should be measured so that there are perfectly free-flowing products. It is preferably 10 to 16% by weight.
- the grain structure of the powder component according to the invention is characteristic and differs considerably from the grain structure in known or commercially available detergents.
- the powder component according to the invention consists predominantly, i.e. more than 50% by weight, preferably more than 60% by weight and in particular 65 to 100% by weight of droplet to rod-shaped particles which have an average diameter of 0.02 to 1.5 mm, preferably from 0.05 to 1 mm and an average length from 0.1 to 5 mm, preferably from 0.3 to 3 mm, a ratio of diameter to length from 1: 1.2 to 1:10, preferably from 1: 1.4 to 1: 8 with a pronounced maximum at 1: 1.8 to 1: 5.
- the particles are compact, i.e. they have a dense structure that is not sponge-like or foam-like. Your surface is closed, i.e. not porous and appears smooth when viewed macroscopically. A surface structure can be seen under the microscope, which can be described as pitted to streaked and reminds of solidified, non-porous slags.
- Figures 1 to 5 show such characteristic particles with increasing magnification.
- Figure 5 shows the front of such a particle in the area of a break. This example shows that the surface structure inside the particles can continue.
- Figures 6 and 7 of a conventional spray powder with a low bulk density attached for comparison show agglomerated particles of irregular, in a first approximation spherical shape and largely smooth surface.
- the interior of the individual particles is inflated, as can be seen from the cross section of a particle shown in Figure 7, and has a porous sponge or foam structure which is characteristic of such spray powder.
- Such powder structures are not the subject of the invention.
- the parameter "to more than 50% by weight” or “preferably 65 to 100% by weight of drop-shaped or rod-shaped particles” means that the agents can also be built up on a subordinate scale from particles of a different shape, i.e. that two or more droplet to rod-shaped particles are cemented into agglomerates of irregular shapes, or that small proportions of approximately spherical particles are produced or that elongated particles break into short fragments during further processing or during transport.
- the detergent component according to the invention can be mixed with additional powder products which have been produced by customary methods and have a different powder spectrum.
- additional powder products which have been produced by customary methods and have a different powder spectrum.
- these powder products also include detergent precursors, so-called compounds, which are composed of anionic sulfonate and / or sulfate surfactants and, if appropriate, soaps, together with carriers such as sodium triphosphate, zeolite A and water glass, and are prepared by conventional spray drying or mixed granulation.
- Textile-softening granules which contain quaternary ammonium compounds as active ingredients together with soluble or insoluble carriers and dispersion inhibitors or which are based on sheet silicates and long-chain tertiary amines are also suitable as additives.
- These additional powder products are made up of differently designed, known particle shapes, for example more or less spherical beads, prills or granules.
- This bulk density is 550 to 800 g / l, preferably 600 to 750 g / l and in particular 620 to 720 g / l.
- the detergent component according to the invention due to its characteristic rod-shaped powder structure, is only suitable to a limited extent for determining the particle size distribution by means of sieve analysis, the particle spectrum can be determined using this method. It shows that the grain spectrum is comparatively narrow, i.e. more than 70 wt .-%, usually even 80 to 90 wt .-% of the powders are within a range between 0.2 and 0.8 mm mesh size. In the case of a conventional spray powder with a low bulk density, this grain size range generally does not account for more than 50 to 70% by weight. The proportion of dust in the powder component according to the invention and the proportion of oversize are accordingly low, so that subsequent sieving of the tower powder or subsequent addition of dust-binding agents is unnecessary.
- the detergent component according to the invention is free-flowing and, in terms of its flowability, exceeds the known, specifically light, sprayed hollow-sphere powder.
- Their pourability can be compared to that of dry sand, namely the pourability which can be carried out according to a test given in the examples is in the order of more than 60%, preferably from 75 to 95%, of that of dry sand with a specific grain specification .
- This good flowability is highly surprising, since one had to expect that the powder particles would lose their ability to roll off with increasing distance from spherical dimensions.
- the agents according to the invention even exceed these Values, ie the volume decreases here are usually below 10% and reach a value of 5% in favorable cases.
- the high volume consistency, combined with the excellent pourability, facilitates in particular precise and reproducible dosing during filling and in use.
- the grains have a coating of a finely divided, water-soluble or dispersible solid as a fluidizing agent in an amount which is 0.01 to 3 wt .-% of the granular Spray product is.
- the finely divided synthetic zeolites of the NaA or NaX type have proven particularly useful as coating agents. The positive effect of these zeolites is not only limited to the improved flowability, but also increases the proportion of builders and thus the washing power of the product.
- Fine-particle silica with a large specific surface area in particular pyrogenic silica (Aerosil®), is also suitable as a fluidizing agent.
- the proportion of the fluidizing agent is preferably 0.1 to 2% by weight in the case of the zeolite, and preferably 0.05 to 0.5% by weight in the case of the finely divided silica, based on the granular spray product.
- powder materials already proposed for powdering sticky detergent granules such as finely divided sodium tripolyphosphate, sodium sulfate, magnesium silicate, talc, bentonite and organic polymers such as carboxymethyl cellulose and urea resins, can also be used, provided that they have a particle size of less than 0.1 mm, for example from 0.001 to 0 , 08 mm.
- Coarse powder provenances such as those usually used in detergents and cleaning agents, have to be comminuted beforehand. Coating agents of this type are preferably used in proportions of 1 to 3% by weight.
- the invention further relates to a method for producing the detergent component according to the invention.
- the production is characterized in that a slurry of the components containing a total of 55 to 35% by weight of water (including the water adsorptively or bound as hydrate) is produced by means of nozzles under a pressure of 16 to 30 bar measured at the nozzle inlet at a ; Sprayed the diameter of the nozzle outlet opening from 3 to 5.5 mm into a drying tower, the ratio of pressure at the nozzle inlet to the diameter of the nozzle outlet opening being 3 to 9 bar / mm.
- Conventional systems can be used to carry out the spray drying process, as are already used for the production of conventional sprayed detergents.
- Such systems usually consist of towers of round cross-section, which are equipped with ring-shaped spray nozzles in the upper part. They also have supply devices for the dry gases as well as dedusting systems for the exhaust air.
- the drying gas is introduced into the lower part of the tower and directed towards the product stream, while in the case of direct current drying, the drying gases are supplied in the top of the drying tower.
- the pressure at the nozzle inlet is preferably 18 to 28 bar and in particular 19 to 25 bar
- the diameter of the nozzle outlet opening is 3.5 to 5 mm
- the ratio of pressure to diameter of the nozzle outlet opening is 4 to 6 bar / mm and in particular 4.5 to 5, 5 bar / mm.
- Compliance with these parameters is decisive for the grain properties of the process products. Significantly exceeding these limits in both directions leads to the formation of more or less irregular to spherical agglomerates with a foam-like structure, in particular when the pressure is increased or the nozzle is narrowed, which results in a lower bulk density and poorer pouring properties. If the pressure is reduced too much, the atomization performance may be poor and crusts may form in the area of the nozzle outlet opening.
- the spray drying system is operated with hot air or hot combustion gases, which are preferably conducted in countercurrent to the spray material.
- the dry gas is expediently introduced tangentially into the tower, which results in a certain swirl effect.
- the inlet temperature of the dry gas should not exceed 250 ° C and should preferably be 180 ° C to 240 ° C, in particular 190 ° C to 220 ° C.
- Operation with hotter dry gases requires the use of predominantly highly ethoxylated or mixed alkoxylated surfactants in order to prevent smoke formation in the exhaust air. If the surfactant mixtures of low and highly ethoxylated compounds disclosed as preferred above are used, there will be no disturbances from smoke formation if the temperature range of 190 ° C to 220 ° C is observed, and the measured exhaust gas values are far below the legal maximum limit.
- the inlet temperature of the drying gas in the spray drying system from 180 ° C to 240 ° C, preferably from 190 ° C to 220 ° C, it should be noted that these are temperatures of the gas in the so-called ring channel of the spray tower.
- the temperature of the gas flowing into the spray zone from this ring channel and coming into contact with the powder is usually 30 ° C. to 40 ° C. lower.
- the temperature of the drying gases when leaving the drying tower is generally 90 ° C. + 15 ° C. and is preferably in the range between 80 ° C. and 95 ° C.
- the upper value can be subject to certain fluctuations, which include depends on the outside temperature. It should be selected so that the dew point is not undercut in the downstream dedusting systems.
- the aqueous batch to be sprayed preferably contains a total of 55 to 42% by weight, preferably 52 to 44% by weight and in particular 50 to 46% by weight of water, which also contains the water bound by adsorption or hydrate.
- Higher water contents are impractical because they increase the degree of hydrolysis of the tripolyphosphate, increase energy consumption and lead to a lower bulk density.
- Lower levels can lead to an excessive increase in the viscosity of the slurry and therefore make special measures such as increasing the mixing and conveying capacity or the addition of viscosity-reducing agents such as toluene, xylene or cumene sulfonate necessary.
- the order in which the slurries are prepared is not critical, processing can be facilitated by adhering to certain process conditions. In addition, it is advisable to keep the mixing and residence times as short as possible due to the sharp increase in viscosity in the slurry batch. It is recommended that the liquid products, i.e. the melted nonionic surfactants and those already in aqueous solution or
- Slurry components present, e.g. to present the aluminosilicate present as a filter-moist paste and, if appropriate, additional water, and to add the anhydrous constituents, in particular the anhydrous or, if appropriate, partially hydrated tripolyphosphate, with vigorous stirring.
- anhydrous, slowly hydrating sodium tripolyphosphate of Form II is used, a strong increase in viscosity and a greater hydrolysis to lower phosphates are avoided, but under certain circumstances a somewhat reduced flowability of the spray product has to be accepted.
- Faster hydrating tripolyphosphate for example one with higher proportions of Form I or partially prehydrated tripolyphosphate, leads to higher slurrie viscosities. It is an advantage of the process that the use of prehydrated polyphosphate is not necessary.
- an anhydrous sodium tripolyphosphate which consists of 30 to 50%, in particular 35 to 45%, of modification I.
- Tripolyphosphate of Form I is known for an increased rate of hydration.
- This increased rate of hydration can pose problems with the processability of the aqueous batch (slurry).
- the hydration removes free water from the slurry, with the result that the viscosity rises sharply.
- an excessive slurry viscosity not only complicates processing, i.e. mixing, conveying and spraying the slurries, but also leads to lower bulk densities in the finished powder.
- the viscosity of the slurry In order to ensure adequate flowability of the slurry and spray products with favorable powder properties, it has proven to be advantageous to adjust the viscosity of the slurry to a range from 2000 to a maximum of 15,000 mPa.s, preferably from 5000 to 12,000 mPa.s and in particular from 6000 to 10,000 mPa.s to set.
- This adjustment is advantageously performed in such a manner that the slurry is heated before the 'addition of the solids, particularly before addition of the tripolyphosphate to temperatures above 85 ° C, for example at 86 ° C to 102 ° C.
- the heating is expediently carried out by introducing steam, in particular superheated steam.
- the hydration of the tripolyphosphate in the slurry is largely prevented or delayed to such an extent that there is no undesirable increase in viscosity within the processing time.
- Keeping the slurry liquid can also be facilitated by applying strong shear forces, for example by intensive mixing by means of an agitator or by means of pumping devices with which the slurry is circulated.
- strong shear forces prevents the formation of structural viscosities.
- the use of viscosity regulators ensures that the preferred viscosity ranges are maintained.
- the product leaving the spray tower generally has a temperature of 65 ° C to 80 ° C. It has been shown that under unfavorable conditions, which are unavoidable in a continuous, long-term production, fluctuations in certain product properties, such as bulk density and pourability of the grains, can occur. Seasonal climate fluctuations can be an influence, for example. In this connection, high air temperatures have proven to be unfavorable in the further processing of the powders, especially in the cooling phase after leaving the spray tower. If the still warm spray material leaving the drying tower is stored in silos for a longer period of time, the nonionic surfactants can migrate to the surface of the spray grains, with the result that their flowability decreases without caking occurring.
- the spray-dried grains can be coated or powdered before, after or expediently at the same time as the addition of further powder components.
- powder components include per-compounds, bleach activators (so-called peracid precursors), enzyme granules, foam inhibitors or foam activators and so-called compounds, i.e. Carrier substances and surfactants, in particular anionic surfactants, or powder products consisting of carrier substances and fabric softeners.
- Water-insoluble coating agents such as zeolite and silica aerogels, can also be used before spray drying is complete, i.e. by blowing into the lower part of the drying tower on the detergent granules already formed.
- the coating agent can be introduced into the tower by metering it into the dry air.
- the powdering of the spray-dried grains leads, among other things, to a partial smoothing of the grain surface, so that the flow behavior of such grains, which already have very good pourability and flowability, is further improved.
- the bulk density of the powders can also be increased slightly as a result, since the coating material apparently enables the grains to be packed more densely.
- the invention thus also encompasses a method for the aftertreatment of the granular, spray-dried powders in a mixing device with 0.01 to 3% by weight of a finely divided solid as defined above.
- Other powder components that can be added to the spray-dried detergents include substances that are unstable under the spray-drying conditions or that lose their specific effect in whole or in part or that would adversely change the properties of the spray-drying product.
- enzymes from the class of proteases, lipases and amylases or their mixtures Enzymes obtained from bacterial strains or fungi, such as Bacillus subtillis, Bacillus licheniformis and Streptomyces griseus, are particularly suitable.
- Fragrances and foam suppressants such as silicones or paraffin hydrocarbons, are also generally added to the spray-dried powder component to avoid loss of effectiveness.
- Suitable bleaching components for admixing are the perhydrates and per-compounds commonly used in washing and bleaching agents.
- the bleach activators include in particular N-acyl compounds.
- suitable N-acyl compounds are polyacylated alkylenediamines, such as tetraacetylmethylene diamine, tetraacetylethylenediamine, and acylated glycolurils, such as tetraacetylglycoluril.
- Further examples are N-alkyl-N-sulfonyl-carbonamides, N-acylhydantoins, N-acylated cyclic triazoles, urazoles, diketopiperazines, sulfurylamides, cyanurates and imidazolines.
- acylated sugars such as glucose pentaacetate are particularly suitable as 0-acyl compounds.
- Preferred bleach activators are tetraacetylethylenediamine and glucose pentaacetate.
- the enzymes, foam-influencing agents and bleach activators can be granulated in a known manner and / or coated with water-soluble or water-dispersible coating substances in order to avoid interactions with the other detergent components during storage of the powdery mixtures.
- Salts which are customary to absorb water of hydration can serve as granulating agents.
- Suitable coating substances are water-soluble polymers, such as polyethylene glycol, cellulose ethers, cellulose esters, water-soluble starch ethers and starch esters, and nonionic surfactants of the alkoxylated alcohol, alkylphenol, fatty acid and fatty acid amide type ....
- the detergent component produced according to the invention is only slightly foam-active and can be used in washing machines without problems.
- the spray-dried powder product is subsequently expanded with foam-active surfactants and surfactant mixtures, preferably in a compound -Form, added.
- foam-active surfactants and surfactant mixtures preferably in a compound -Form, added.
- foam-active surfactants and surfactant mixtures preferably in a compound -Form, added.
- foam-active surfactants and surfactant mixtures preferably in a compound -Form
- foam-active surfactants and surfactant mixtures preferably in a compound -Form
- foam-active surfactants and surfactant mixtures preferably in a compound -Form, added.
- anionic surfactants of the sulfonate and sulfate type as well as zwitterionic surfactants.
- Such an addition can also lead to a further increase in washing power.
- Their addition can be up to 10% by
- Alkylbenzenesulfonates for example n-dodecylbenzenesulfonate, olefin sulfonates, alkanesulfonates, primary or secondary alkyl sulfates, sulfo fatty acid esters as well as sulfates of ethoxylated or propoxylated higher molecular weight alcohols, monoalkylated or dialkylated sulfosuccinates, sulfuric acid esters of fatty acid partial esters, and fatty acid partial esters of glyceryl fatty acid.
- Suitable zwitterionic surfactants are alkyl betaines and especially alkyl sulfone betaines, e.g. the 3- (N, N-dimethyl-N-alkylammonium) propane-1-sulfonate and 2-hydroxypropane-1-sulfonate.
- alkylbenzenesulfonates, olefin sulfonates, alkanesulfonates, fatty alcohol sulfates, ⁇ -sulfofatty acid esters are to be regarded as preferred because of their foam-raising and washing-enhancing action. If emphasis is primarily placed on foam activation, the use of sulfates of ethoxylated fatty alcohols, in particular 1 to 3 glycol ether groups, and alkylsulfobetaines is recommended.
- the anionic surfactants or mixtures thereof are preferably in the form of the sodium or potassium salts and as salts of organic bases, such as mono-, di- or triethanolamine. If the anionic and zwitterionic compounds mentioned have an aliphatic hydrocarbon radical, this should preferably be straight-chain and have 8 to 20, in particular 12 to 18, carbon atoms. In the compounds having an araliphatic hydrocarbon radical, the preferably unbranched alkyl chains contain an average of 6 to 16, in particular 8 to 14, carbon atoms.
- the additional optional anionic and zwitterionic surfactants are also expediently used in granular form.
- the usual inorganic salts such as sodium sulfate, sodium carbonate, phosphates and zeolites, and mixtures thereof are used as granulation aids or carrier substances.
- Fabric softening additives generally consist of granules containing a softening quaternary ammonium compound (QAV), e.g. Distearyldimethylammonium chloride, a carrier and an additive which delays the dispersion in the wash liquor.
- QAV softening quaternary ammonium compound
- a typical such granulate is e.g. polydimethylsiloxane activated from 86% by weight of QAV, 10% by weight of pyrogenic silica and 4% by weight of silicone oil (with pyrogenic silica); another granulate has the composition 30% by weight QAV, 20% by weight sodium triphosphate, 20% by weight zeolite NaA, 15% by weight water glass, 2% by weight silicone oil and the rest water.
- the additional powder components generally do not exceed a proportion of 10 to 40% by weight, preferably 30 to 30% by weight (based on the finished mixture), the influence of the additives on the powder properties generally remains small.
- the sodium hydroxide as 50% sodium hydroxide solution, the molten ethoxylates and the sodium silicate in 36% aqueous solution were initially introduced, then the aluminosilicate (54% water) present as a filter-moist paste and the other constituents, predominantly present in aqueous solution, and finally that anhydrous phosphate added.
- the slurry had a total water content of 48.2%, a temperature of 90 ° C and a viscosity of 8500 mPa.s after homogenization under a pressure of 20 bar measured at the nozzle inlet, sprayed through swirl nozzles with an outlet opening of 4 mm in a spray tower.
- the dry gas introduced in countercurrent under swirl had an inlet temperature of 220 ° C and an outlet temperature (measured at the filter inlet) of 90 ° C.
- the dust explosion limit was not reached at a powder concentration between 30 and 200 g / m, ie the product is classified in dust explosion class 0.
- the smoke meter at the outlet of the exhaust air filter shows a deflection between 0.02 and 0.08 scale parts (permissible limit 0.15 scale parts), ie critical smoke formation was not achieved.
- the spray product After leaving the spray tower, the spray product had a temperature of 70 ° C. and was cooled to a temperature of 28 ° C. in less than 1 minute in a pneumatic conveyor system. It consisted of over 75% by weight of elongated, i.e. rod-like to droplet-shaped particles with an average length of 0.8 to 3 mm and an average diameter of 0.1 to 0.6 mm with an average ratio of diameter to length of 1: 1.5 to 1: 6 The rest consisted of irregular sticky particles and small amounts of dust cemented together. The coarse content (1.6-3 mm) was less than 1% by weight. The bulk density of the powder was 650 g / 1.
- Dry sea sand with the following grain spectrum was chosen as the reference substance.
- the mixture proved to be a high-quality detergent that can be used in the temperature range between 30 ° and 100 ° C.
- the flushability and the formation of residues in the input devices of fully automatic washing machines no differences between a loose spray powder and the test product were recognizable.
- the solution properties of the comparison product listed under (d) were poorer, which led to the formation of residues in the induction device and on the textiles.
- test V the smoke measuring device showed a scale value of 2 divisions, which means that the smoke emission is above the permissible limit.
- the slurry was sprayed into a spray tower at a pressure of 22 bar via swirl nozzles with an outlet opening of 4.1 mm.
- the air conducted in countercurrent had an inlet temperature (measured before entering the ring channel) of 218 ° C and an initial temperature of 89.5 ° C.
- the smoke indicator in the exhaust air was 0.02 to 0.07 divisions, with regard to the powder concentration in the drying tower the same conditions as in example 1 prevailed.
- the powder leaving the spray tower was brought to 30 ° C. in the delivery shaft with flowing, 24 ° C. warm outside air cooled down.
- the spray product consisted of over 60% by weight of rod-shaped particles with an average length of 0.7 to 2.7 mm and an average diameter of 0.1 to 0.7 mm with a dimension ratio of 1: 1.6 to 1 : 5 and a dust content of less than 1% by weight.
- the bulk density was 645 g / 1 and the flow rate was 83%.
- the spray product was dusted with 1.4% by weight of dry, finely crystalline aluminosilicate (zeolite NaA, particle size 0.5 to 7 pm) in a continuously operated mixer while simultaneously adding 10% by weight of sodium perborate. After admixing 1% by weight of enzyme granules and 3% by weight of granulated bleach activator (tetraacetylethylene diamine), the bulk density rose to 690 g / 1 with a free-flowing capacity of 88%. The solution properties in water were still good.
- Example 1 was repeated, but instead of the sodium tripolyphosphate used there, one containing 40% Form I was used. Before the phosphate was added, the slurry was heated to a temperature of 90 ° C. and then pumped through a homogenizer in a circuit. The viscosity was 11,000 mPa.s with a water content of 43% by weight. The spraying was carried out at a pressure of 22 bar and a nozzle opening of 4.0 mm. The temperature of the counter-current dry air was 215 ° C at the tower entrance and 89 ° C at the tower exit. The remaining process parameters were the same as in Example 1.
- the spray product corresponded to the powder according to Example 1 in terms of particle size and bulk density.
- the pourability was 86% of that of dry sand.
- Aftertreatment with 0.06% by weight of silica airgel (Aerosil) improved the flowability to 89% of that of dry sand and led to an increase in the bulk density from 640 g / 1 to 660 g / 1.
- Example 2 was repeated, but the temperature of the cooling air flowing into the conveyor system was 37 ° C. due to high outside temperatures. Due to the delayed cooling of the powder, which was still warm from the spraying process, there was a slight exudation of nonionic Surfactant on the surface of the detergent granules with the result that the pourability of the powder to 81%. a bulk weight of 620 g / 1 dropped. After-treatment with 1% by weight of NaA zeolite (particle size 1 to 8 ⁇ m) in a continuously operating mixer increased the free-flowing capacity to 86% of that of dry sand and the bulk density to 640 g / l.
- the viscosity was measured with a convection-type rotary viscometer from Brabender, Duisburg, Federal Republic of Germany.
- 89 parts by weight of the spray product from Example 1 were mixed with 1 part by weight of enzyme granules and 10 parts by weight of a surfactant compound in a continuously operated mixer.
- the surfactant compound was produced by spray mixing with the following composition:
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- 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)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT84103320T ATE35692T1 (de) | 1983-03-25 | 1984-03-26 | Koernige, freifliessende waschmittelkomponente und verfahren zu ihrer herstellung. |
Applications Claiming Priority (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3310906 | 1983-03-25 | ||
DE3310906 | 1983-03-25 | ||
US54156983A | 1983-10-13 | 1983-10-13 | |
DE3344698 | 1983-12-10 | ||
DE3344698 | 1983-12-10 | ||
US541569 | 1990-06-21 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0120492A2 true EP0120492A2 (fr) | 1984-10-03 |
EP0120492A3 EP0120492A3 (en) | 1986-02-19 |
EP0120492B1 EP0120492B1 (fr) | 1988-07-13 |
Family
ID=27190870
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP84103320A Expired EP0120492B1 (fr) | 1983-03-25 | 1984-03-26 | Composante granuleuse de détergent, à écoulement libre et procédé pour sa préparation |
Country Status (5)
Country | Link |
---|---|
EP (1) | EP0120492B1 (fr) |
BR (1) | BR8406459A (fr) |
DE (1) | DE3472682D1 (fr) |
DK (1) | DK161842C (fr) |
WO (1) | WO1984003708A1 (fr) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0167916A2 (fr) * | 1984-07-02 | 1986-01-15 | Henkel Kommanditgesellschaft auf Aktien | Procédé de préparation d'un adjuvant de détergent non ionique séché par pulvérisation |
EP0179264A1 (fr) * | 1984-09-22 | 1986-04-30 | Henkel Kommanditgesellschaft auf Aktien | Procédé pour la production d'une composante de lavage granulaire à écoulement libre |
EP0327963A2 (fr) * | 1988-02-10 | 1989-08-16 | Henkel Kommanditgesellschaft auf Aktien | Procédé pour augmenter la densité de détergents séchés par vaporisation |
EP0337330A2 (fr) * | 1988-04-15 | 1989-10-18 | Henkel Kommanditgesellschaft auf Aktien | Procédé pour augmenter la densité des détergents séchés par pulvérisation et contenant peu de phosphate |
GB2231579A (en) * | 1989-05-09 | 1990-11-21 | Unilever Plc | Spray-dried detergent |
WO1995007339A1 (fr) * | 1993-09-04 | 1995-03-16 | Henkel Kommanditgesellschaft Auf Aktien | Granule seche par pulverisation a masse volumique apparente elevee |
EP0820762A1 (fr) | 1996-07-15 | 1998-01-28 | Unilever Plc | Compositions de parfums |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE69422675T3 (de) * | 1993-09-13 | 2008-05-21 | The Procter & Gamble Company, Cincinnati | Granuläre Waschmittelzusammensetzungen, umfassend nichtionisches Tensid, und Verfahren zur Herstellung solcher Zusammensetzungen |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1579247A (fr) * | 1967-09-04 | 1969-08-22 | ||
DE2724349A1 (de) * | 1977-05-28 | 1978-12-07 | Henkel Kgaa | Verfahren zur herstellung spruehgetrockneter, nichtionische tenside enthaltender waschmittel |
JPS5562999A (en) * | 1978-11-07 | 1980-05-12 | Kawaken Fine Chemicals Co | Spray dry detergent composition |
GB2082620A (en) * | 1977-10-06 | 1982-03-10 | Colgate Palmolive Co | Detergent compositions |
-
1984
- 1984-03-26 WO PCT/EP1984/000085 patent/WO1984003708A1/fr unknown
- 1984-03-26 BR BR8406459A patent/BR8406459A/pt not_active IP Right Cessation
- 1984-03-26 DE DE8484103320T patent/DE3472682D1/de not_active Expired
- 1984-03-26 EP EP84103320A patent/EP0120492B1/fr not_active Expired
- 1984-11-21 DK DK553084A patent/DK161842C/da not_active IP Right Cessation
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR1579247A (fr) * | 1967-09-04 | 1969-08-22 | ||
DE2724349A1 (de) * | 1977-05-28 | 1978-12-07 | Henkel Kgaa | Verfahren zur herstellung spruehgetrockneter, nichtionische tenside enthaltender waschmittel |
GB2082620A (en) * | 1977-10-06 | 1982-03-10 | Colgate Palmolive Co | Detergent compositions |
JPS5562999A (en) * | 1978-11-07 | 1980-05-12 | Kawaken Fine Chemicals Co | Spray dry detergent composition |
Non-Patent Citations (1)
Title |
---|
CHEMICAL ABSTRACTS, Band 93, Nr. 10, September 1980, Seite 117, Ref.Nr. 97309p, Columbus, Ohio, US; & JP - A - 80 62 999 (KAWAKEN FINE CHEMICALS CO. LTD.) 12.05.1980 * |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0167916A2 (fr) * | 1984-07-02 | 1986-01-15 | Henkel Kommanditgesellschaft auf Aktien | Procédé de préparation d'un adjuvant de détergent non ionique séché par pulvérisation |
EP0167916A3 (fr) * | 1984-07-02 | 1987-07-01 | Henkel Kommanditgesellschaft auf Aktien | Procédé de préparation d'un adjuvant de détergent non ionique séché par pulvérisation |
EP0179264A1 (fr) * | 1984-09-22 | 1986-04-30 | Henkel Kommanditgesellschaft auf Aktien | Procédé pour la production d'une composante de lavage granulaire à écoulement libre |
EP0327963A2 (fr) * | 1988-02-10 | 1989-08-16 | Henkel Kommanditgesellschaft auf Aktien | Procédé pour augmenter la densité de détergents séchés par vaporisation |
EP0327963A3 (fr) * | 1988-02-10 | 1990-04-11 | Henkel Kommanditgesellschaft auf Aktien | Procédé pour augmenter la densité de détergents séchés par vaporisation |
EP0337330A2 (fr) * | 1988-04-15 | 1989-10-18 | Henkel Kommanditgesellschaft auf Aktien | Procédé pour augmenter la densité des détergents séchés par pulvérisation et contenant peu de phosphate |
EP0337330A3 (en) * | 1988-04-15 | 1990-04-11 | Henkel Kommanditgesellschaft Auf Aktien | Process for increasing the density of spray-dried detergents with a reduced phosphate content |
GB2231579A (en) * | 1989-05-09 | 1990-11-21 | Unilever Plc | Spray-dried detergent |
WO1995007339A1 (fr) * | 1993-09-04 | 1995-03-16 | Henkel Kommanditgesellschaft Auf Aktien | Granule seche par pulverisation a masse volumique apparente elevee |
US5767057A (en) * | 1993-09-04 | 1998-06-16 | Henkel-Ecolab Gmbh & Co. Ohg | Spray-dried granules of high apparent density |
EP0820762A1 (fr) | 1996-07-15 | 1998-01-28 | Unilever Plc | Compositions de parfums |
Also Published As
Publication number | Publication date |
---|---|
DK161842B (da) | 1991-08-19 |
DK161842C (da) | 1992-01-27 |
EP0120492B1 (fr) | 1988-07-13 |
BR8406459A (pt) | 1985-03-12 |
DK553084D0 (da) | 1984-11-21 |
WO1984003708A1 (fr) | 1984-09-27 |
DE3472682D1 (en) | 1988-08-18 |
EP0120492A3 (en) | 1986-02-19 |
DK553084A (da) | 1984-11-21 |
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