WO1998004669A1 - PREPARATION OF LOW lDENSITY DETERGENT AGGLOMERATES CONTAINING SILICA - Google Patents
PREPARATION OF LOW lDENSITY DETERGENT AGGLOMERATES CONTAINING SILICA Download PDFInfo
- Publication number
- WO1998004669A1 WO1998004669A1 PCT/US1997/011985 US9711985W WO9804669A1 WO 1998004669 A1 WO1998004669 A1 WO 1998004669A1 US 9711985 W US9711985 W US 9711985W WO 9804669 A1 WO9804669 A1 WO 9804669A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- detergent
- agglomerates
- silica
- density
- process according
- Prior art date
Links
- 239000003599 detergent Substances 0.000 title claims abstract description 136
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 74
- 230000008569 process Effects 0.000 claims abstract description 68
- 239000000463 material Substances 0.000 claims abstract description 57
- 239000000203 mixture Substances 0.000 claims abstract description 46
- 239000004094 surface-active agent Substances 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 15
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 150000004760 silicates Chemical class 0.000 claims description 6
- 229910021485 fumed silica Inorganic materials 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 230000002209 hydrophobic effect Effects 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 3
- 239000005909 Kieselgur Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 description 28
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 20
- 239000008187 granular material Substances 0.000 description 17
- 238000005342 ion exchange Methods 0.000 description 16
- 239000004615 ingredient Substances 0.000 description 14
- -1 oleyl sulfate Chemical compound 0.000 description 13
- 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 12
- 239000011734 sodium Substances 0.000 description 12
- 238000005054 agglomeration Methods 0.000 description 11
- 230000002776 aggregation Effects 0.000 description 11
- 229910052708 sodium Inorganic materials 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
- 239000012530 fluid Substances 0.000 description 9
- 239000004115 Sodium Silicate Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 229920005646 polycarboxylate Polymers 0.000 description 7
- 235000019351 sodium silicates Nutrition 0.000 description 7
- 238000001694 spray drying Methods 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 235000019832 sodium triphosphate Nutrition 0.000 description 6
- 229910021536 Zeolite Inorganic materials 0.000 description 5
- 239000003945 anionic surfactant Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 229910001424 calcium ion Inorganic materials 0.000 description 5
- 150000007942 carboxylates Chemical class 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000010457 zeolite Substances 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical group [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 4
- 229930182556 Polyacetal Natural products 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 239000002736 nonionic surfactant Substances 0.000 description 4
- 229920006324 polyoxymethylene Polymers 0.000 description 4
- 235000017550 sodium carbonate Nutrition 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical class C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 150000001340 alkali metals Chemical class 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 159000000001 potassium salts Chemical class 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000344 soap Substances 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 238000006677 Appel reaction Methods 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical class CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical group [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 2
- 101710194948 Protein phosphatase PhpP Proteins 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 235000010216 calcium carbonate Nutrition 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Chemical group 0.000 description 2
- 229910052739 hydrogen Chemical group 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229910001425 magnesium ion Chemical group 0.000 description 2
- YDSWCNNOKPMOTP-UHFFFAOYSA-N mellitic acid Chemical class OC(=O)C1=C(C(O)=O)C(C(O)=O)=C(C(O)=O)C(C(O)=O)=C1C(O)=O YDSWCNNOKPMOTP-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 239000002304 perfume Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 229910021647 smectite Inorganic materials 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 150000003871 sulfonates Chemical class 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910009112 xH2O Inorganic materials 0.000 description 2
- 239000001124 (E)-prop-1-ene-1,2,3-tricarboxylic acid Substances 0.000 description 1
- CFPOJWPDQWJEMO-UHFFFAOYSA-N 2-(1,2-dicarboxyethoxy)butanedioic acid Chemical class OC(=O)CC(C(O)=O)OC(C(O)=O)CC(O)=O CFPOJWPDQWJEMO-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- PSZAEHPBBUYICS-UHFFFAOYSA-N 2-methylidenepropanedioic acid Chemical compound OC(=O)C(=C)C(O)=O PSZAEHPBBUYICS-UHFFFAOYSA-N 0.000 description 1
- XYJLPCAKKYOLGU-UHFFFAOYSA-N 2-phosphonoethylphosphonic acid Chemical class OP(O)(=O)CCP(O)(O)=O XYJLPCAKKYOLGU-UHFFFAOYSA-N 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RKWGIWYCVPQPMF-UHFFFAOYSA-N Chloropropamide Chemical compound CCCNC(=O)NS(=O)(=O)C1=CC=C(Cl)C=C1 RKWGIWYCVPQPMF-UHFFFAOYSA-N 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical class OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- SXKQTYJLWWQUKA-UHFFFAOYSA-N O.O.O.O.O.O.O.O.O.O.OB(O)O.OB(O)O.OB(O)O.OB(O)O Chemical compound O.O.O.O.O.O.O.O.O.O.OB(O)O.OB(O)O.OB(O)O.OB(O)O SXKQTYJLWWQUKA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical class OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920000388 Polyphosphate Chemical class 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- ZUBJEHHGZYTRPH-KTKRTIGZSA-N [(z)-octadec-9-enyl] hydrogen sulfate Chemical compound CCCCCCCC\C=C/CCCCCCCCOS(O)(=O)=O ZUBJEHHGZYTRPH-KTKRTIGZSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229940091181 aconitic acid Drugs 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical class [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229920006318 anionic polymer Polymers 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- CMFFZBGFNICZIS-UHFFFAOYSA-N butanedioic acid;2,3-dihydroxybutanedioic acid Chemical compound OC(=O)CCC(O)=O.OC(=O)CCC(O)=O.OC(=O)C(O)C(O)C(O)=O CMFFZBGFNICZIS-UHFFFAOYSA-N 0.000 description 1
- HXDRSFFFXJISME-UHFFFAOYSA-N butanedioic acid;2,3-dihydroxybutanedioic acid Chemical compound OC(=O)CCC(O)=O.OC(=O)C(O)C(O)C(O)=O HXDRSFFFXJISME-UHFFFAOYSA-N 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- GTZCVFVGUGFEME-IWQZZHSRSA-N cis-aconitic acid Chemical compound OC(=O)C\C(C(O)=O)=C\C(O)=O GTZCVFVGUGFEME-IWQZZHSRSA-N 0.000 description 1
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 description 1
- 229940018557 citraconic acid Drugs 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000280 densification Methods 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
- 235000011180 diphosphates Nutrition 0.000 description 1
- 238000004851 dishwashing Methods 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 229960001484 edetic acid Drugs 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- UZABCLFSICXBCM-UHFFFAOYSA-N ethoxy hydrogen sulfate Chemical class CCOOS(O)(=O)=O UZABCLFSICXBCM-UHFFFAOYSA-N 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 229960002598 fumaric acid Drugs 0.000 description 1
- 230000002070 germicidal effect Effects 0.000 description 1
- 229910052816 inorganic phosphate Inorganic materials 0.000 description 1
- 238000004900 laundering Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 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
- 230000007246 mechanism Effects 0.000 description 1
- HNEGQIOMVPPMNR-NSCUHMNNSA-N mesaconic acid Chemical compound OC(=O)C(/C)=C/C(O)=O HNEGQIOMVPPMNR-NSCUHMNNSA-N 0.000 description 1
- 125000005341 metaphosphate group Chemical group 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- HNEGQIOMVPPMNR-UHFFFAOYSA-N methylfumaric acid Natural products OC(=O)C(C)=CC(O)=O HNEGQIOMVPPMNR-UHFFFAOYSA-N 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- CQDGTJPVBWZJAZ-UHFFFAOYSA-N monoethyl carbonate Chemical class CCOC(O)=O CQDGTJPVBWZJAZ-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
- 150000001282 organosilanes Chemical class 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 239000001205 polyphosphate Chemical class 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002002 slurry 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
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- GTZCVFVGUGFEME-UHFFFAOYSA-N trans-aconitic acid Natural products OC(=O)CC(C(O)=O)=CC(O)=O GTZCVFVGUGFEME-UHFFFAOYSA-N 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000012855 volatile organic compound 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
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
-
- 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
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
-
- 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
Definitions
- the present invention generally relates to a process for producing a low density detergent composition. More particularly, the invention is directed to a process during which low density detergent agglomerates are produced by feeding a surfactant paste and dry starting detergent material which includes a silica material into a high speed mixer followed by a drying apparatus. The process produces a free flowing, low density detergent composition which can be commercially sold as a conventional non-compact detergent composition or used as an admix in a low dosage, "compact" detergent product.
- the first type of process involves spray-drying an aqueous detergent slurry in a spray-drying tower to produce highly porous detergent granules.
- the various detergent components are dry mixed after which they are agglomerated with a binder such as a nonionic or anionic surfactant.
- a binder such as a nonionic or anionic surfactant.
- the present invention meets the aforementioned needs in the art by providing a process which produces a low density (less than about 500 g/1) detergent composition directly from starting ingredients such as a surfactant paste and dry detergent ingredients.
- the dry ingredients include a silica material which ultimately is agglomerated such that it forms part of or is in the agglomerate particles themselves rather than "coated" on the outer surface of the agglomerates.
- this provides a low density agglomerate composition having improved physical properties.
- the process does not use the conventional spray drying towers currently used and is therefore more efficient, economical and flexible with regard to the variety of detergent compositions which can be produced in the process Moreover, the process is more amenable to environmental concerns in that it does not use spray drying towers which typically emit particulates and volatile organic compounds into the atmosphere.
- agglomerates refers to particles formed by agglomerating detergent granules or particles which typically have a smaller mean particle size than the formed agglomerates. All percentages used herein are expressed as “percent-by-weight” unless indicated otherwise. All viscosities described herein are measured at 70°C and at shear rates between about 10 to 50 sec " -, preferably at 25 sec ⁇ l . All documents cited herein are incorporated herein by reference.
- a process for preparing low density detergent agglomerates having a density of below about 500 g 1 comprises the steps of: (a) agglomerating a detergent surfactant paste and dry starting detergent material in a high speed mixer to obtain detergent agglomerates, wherein the dry starting detergent material includes a silica material; and (b) drying the detergent agglomerates so as to form the detergent composition having a density of less than about 600 g 1.
- another process for preparing low density detergent agglomerates having a density of below about 500 g 1 comprises the steps of: (a) agglomerating a detergent surfactant paste and dry starting detergent material in a high speed mixer to obtain detergent agglomerates, wherein the dry starting detergent material includes a fumed silica material; (b) mixing the detergent agglomerates in a moderate speed mixer to further agglomerate the detergent agglomerates; and (c) drying the detergent agglomerates so as to form the low density detergent composition having a density of less than about 500 g/1.
- the low density detergent composition made by any of the process embodiments described herein is also provided.
- the present invention is directed to a process which produces free flowing, low density detergent agglomerates having a density of below about 500 g/1, preferably from about 350 g/1 to about 500 g/1.
- the process produces low density detergent agglomerates from a highly viscous surfactant paste having a relatively high water content, typically at least about 10%.
- the present process is used in the production of normal as opposed to low dosage detergents whereby the resulting detergent agglomerates can be used as a detergent or as a detergent additive. It should be understood that the process described herein can be continuous or batch depending upon the desired application.
- starting detergent materials are fed into a mixer for agglomeration.
- the agglomeration step is carried forth initially in a high speed mixer after which an optional moderate speed mixer may follow if further agglomeration is desired.
- the starting detergent materials preferably include a highly viscous surfactant paste and dry detergent material, the components of which are described more fully hereinafter.
- the starting detergent materials are agglomerated in the presence of a silica material as described more fully hereinafter to produce agglomerate particles having the desired low density.
- the instant process preferably entails mixing from about 1% to about 20%, more preferably from about 3% to about 10%, and most preferably from about 3% to about 5%, by weight of a silica material into the high speed mixer.
- the nature and composition of the entering or starting detergent materials and optional adjunct ingredients can vary as described in detail hereinafter.
- silica in the agglomerate rather than as a coating agent, a low density agglomerate can be formed. This is contrary to expectations since using silica as a coating or dusting agent to such that it is deposited on the outer surface of agglomerate particles will raise or increase the density.
- silica inside the agglomerate particles lowers the density as is desired for producing a low density agglomerated composition.
- the silica when subjected agglomeration with a surfactant and subsequent drying step forms a hollow "finger-like" structure inside the individual agglomerate particles, thereby increasing the internal void space in each agglomerate particle. This, of course, results in more porous agglomerates having a relatively low density.
- the other essential step in the process involves drying the agglomerates exiting the high speed mixer or moderate speed mixer if it is optionally used.
- This can be completed in a wide variety of apparatus including but not limited to fluid bed dryers.
- the drying step enhances the.free flowability of the agglomerates and facilities the "fluffy " or "puffy" physical characteristics of the resulting agglomerates. Accordingly, sufficient drying must occur in order to produce the desired low density agglomerates.
- the drying temperature used in the whichever drying apparatus will preferably be from about 50 °C to about 300 °C, more preferably from about 80 °C to about 250 °C, and most preferably, from about 100 °C to about 250 °C
- the mean residence time of the starting detergent materials in the high speed mixer is from about 2 to 45 seconds while the residence time in the optional low or moderate speed mixer (e.g. Lodige Recycler KM 300 "Ploughshare" or other similar equipment) is from about 0.5 to 15 minutes.
- the detergent agglomerates produced by the process preferably have a surfactant level of from about 20% to about 55%, more preferably from about 35% to about 55% and, most preferably from about 45% to about 55%.
- the particle porosity of the resulting detergent agglomerates produced according to the process of the invention is preferably in a range from about 5% to about 50%, more preferably at about 25%.
- an attribute of dense or densified agglomerates is the relative particle size.
- the present process typically provides detergent agglomerates having a mean particle size of from about 250 microns to about 1000 microns, and more preferably from about 400 microns to about 600 microns.
- mean particle size refers to individual agglomerates and not individual particles or detergent granules.
- the combination of the above-referenced porosity and particle size results in agglomerates having density values of below 500 g/1.
- Such a feature is especially useful in the production of laundry detergents having varying dosage levels as well as other granular compositions such as dishwashing compositions.
- the detergent agglomerates exiting the fluid bed dryer are further conditioned by cooling the agglomerates in a fluid bed cooler or similar apparatus as are well known in the art.
- Another optional process step involves adding a coating agent to improve flowability and/or minimize over agglomeration of the detergent composition in one or more of the following locations of the instant process: (1) the coating agent can be added directly after the fluid bed cooler ; (2) the coating agent may be added between the fluid bed dryer and the fluid bed cooler; (3) the coating agent may be added between the fluid bed dryer and the moderate speed mixer; and/or (4) the coating agent may be added directly to the moderate speed mixer and the fluid bed dryer.
- the coating agent is preferably selected from the group consisting of aluminosilicates, silicates, carbonates and mixtures thereof.
- the coating agent not only enhances the free flowability of the resulting detergent composition which is desirable by consumers in that it permits easy scooping of detergent during use, but also serves to control agglomeration by preventing or minimizing over agglomeration, especially when added directly to the optional moderate speed mixer. As those skilled in the art are well aware, over agglomeration can lead to very undesirable flow properties and aesthetics of the final detergent product.
- the process can comprise the step of spraying an additional binder in one or both of the mixer or fluid bed dryers.
- a binder is added for purposes of enhancing agglomeration by providing a "binding" or "sticking" agent for the detergent components.
- the binder is preferably selected from the group consisting of water, anionic surfactants, nonionic surfactants, polyethylene glycol, polyvinyl pyrrolidone polyacrylates, citric acid and mixtures thereof.
- suitable binder materials including those listed herein are described in Beerse et al, U.S. Patent No. 5,108,646 (Procter & Gamble Co.), the disclosure of which is incorporated herein by reference.
- optional steps contemplated by the present process include screening the oversized detergent agglomerates in a screening apparatus which can take a variety of forms including but not limited to conventional screens chosen for the desired particle size of the finished detergent product.
- Other optional steps include conditioning of the detergent agglomerates by subjecting the agglomerates to additional drying in the one of the aforementioned drying apparatus.
- agglomerates exiting the moderate speed mixer can be dried in a spray drying tower as described in Capeci et al, U.S. Patent 5,496,487 (Procter & Gamble).
- Another optional step of the instant process entails finishing the resulting detergent agglomerates by a variety of processes including spraying and/or admixing other conventional detergent ingredients.
- the finishing step encompasses spraying perfumes, brighteners and enzymes onto the finished agglomerates to provide a more complete detergent composition.
- Such techniques and ingredients are well known in the art.
- the detergent surfactant paste used in the process is preferably in the form of an aqueous viscous paste, although forms are also contemplated by the invention.
- This so-called viscous surfactant paste has a viscosity of from about 5,000 cps to about 100,000 cps, more preferably from about 10,000 cps to about 80,000 cps, and contains at least about 10% water, more preferably at least about 20% water The viscosity is measured at 70°C and at shear rates of about 10 to 100 sec. * '' .
- the surfactant paste if used, preferably comprises a detersive surfactant in the amounts specified previously and the balance water and other conventional detergent ingredients.
- the surfactant itself, in the viscous surfactant paste, is preferably selected from anionic, nonionic, zwitterionic, ampholytic and cationic classes and compatible mixtures thereof.
- Detergent surfactants useful herein are described in U.S. Patent 3,664,961, Norris, issued May 23, 1972, and in U.S. Patent 3,919,678, Laughlin et al., issued December 30, 1975, both of which are incorporated herein by reference.
- Useful cationic surfactants also include those described in U.S. Patent 4,222,905, Cockrell, issued September 16, 1980, and in U.S. Patent 4,239,659, Murphy, issued December 16, 1980, both of which are also incorporated herein by reference.
- anionics and nonionics are preferred and anionics are most preferred.
- Nonlimiting examples of the preferred anionic surfactants useful in the surfactant paste include the conventional C j i-Cjg alkyl benzene sulfonates ("LAS"), primary, branched-chain and random C10-C20 alkyl sulfates (“AS”), the C j r j -Cig secondary (2,3) alkyl sulfates of the formula CH3(CH2) x (CHOSO3 ⁇ M + ) CH3 and CH3 (CH2) y (CHOSO 3 " M + ) CH2CH3 where x and (y + 1) are integers of at least about 7, preferably at least about 9, and M is a water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, and the Cio-Cj g alkyl alkoxy sulfates ("AE X S”; especially EO 1-7 ethoxy sulfates).
- LAS C j i-C
- exemplary surfactants useful in the paste of the invention include and Cjo-Cig alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the C 1 Q- 18 glycerol ethers, the C ⁇ Q-C ⁇ alkyl polyglycosides and their corresponding sulfated polyglycosides, and C ] 2*C ⁇ g alpha-sulfonated fatty acid esters.
- the conventional nonionic and amphoteric surfactants such as the Cj2-Ci8 alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and Cg-C ⁇ alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxy/propoxy), C ⁇ -Cj betaines and sulfobetaines ("sultaines"), CjQ-Ci g amine oxides, and the like, can also be included in the overall compositions.
- the C10-C18 N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C 12-C 1 g N-methylglucamides. See WO 9,206, 154.
- sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C j Q-C ⁇ g N- (3-methoxypropyl) glucamide.
- the N-propyl through N-hexyl C]2-C]g glucamides can be used for low sudsing.
- C10-C20 conventional soaps may also be used. If high sudsing is desired, the branched-chain C JO-C I ⁇ soaps may be used. Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are listed in standard texts.
- the starting dry detergent material of the present process preferably comprises a silica material.
- Silica is highly dispersed amorphous silicon dioxide that is commercially available in many forms. Most commonly, silica has a tapped density of from 50 g/1 to 120 g/1. The specific surface area of the particles ranges from 25 square meters per gram to 800 square meters per gram.
- the surface of the silica particles can be chemically modified to change their behavior with respect to water. For example, silica particles may be treated with organosilanes to make the particles predominantly hydrophobic. It has been found that silicas that are hydrophobic in nature work extremely well in the current process invention; however, hydrophilic silicas are useful in the process, as well. Additionally, diatomaceous earth materials may be used in conjunction with, or as a substitute for, the silicas mentioned herein.
- silicas are usually prepared by one of two techniques; either by precipitation (i.e. precipitated silicas) or by high temperature flame hydrolysis (i.e. fumed silicas). Both precipitated silicas and fumed silicas are useful in the current invention.
- Precipitated silicas generally have an agglomerate size of from 3 micrometers to 100 micrometers, whereas fumed silicas made by flame hydrolysis usually have particles which are substantially spherical and have an average particle diameter of from about 7 nm to about 40 nm. Fumed silicas having an average particle size of from about 7 to about 25 nm are preferred in the present invention.
- Exemplary commercially available silicas useful in the process invention include those supplied by Degussa AG (Germany) identified as AerosilTM, and particularly preferred is AerosilTM R927. Silicas which are hydrophobic, fumed and have surface areas of at least about 1 10 square meters per gram and an average particle diameter size of 16 nm are most preferred.
- the dry detergent material also preferably includes a detergent aluminosilicate builder which are referenced as aluminosilicate ion exchange materials.
- the aluminosilicate ion exchange materials used herein as a detergent builder preferably have both a high calcium ion exchange capacity and a high exchange rate Without intending to be limited by theory, it is believed that such high calcium ion exchange rate and capacity are a function of several interrelated factors which derive from the method by which the aluminosilicate ion exchange material is produced.
- the aluminosilicate ion exchange materials used herein are preferably produced in accordance with Corkill et al, U.S. Patent No. 4,605,509 (Procter & Gamble), the disclosure of which is incorporated herein by reference.
- the aluminosilicate ion exchange material is in "sodium" form since the potassium and hydrogen forms of the instant aluminosilicate do not exhibit the as high of an exchange rate and capacity as provided by the sodium form.
- the aluminosilicate ion exchange material preferably is in over dried form so as to facilitate production of crisp detergent agglomerates as described herein.
- the aluminosilicate ion exchange materials used herein preferably have particle size diameters which optimize their effectiveness as detergent builders.
- particle size diameter represents the average particle size diameter of a given aluminosilicate ion exchange material as determined by conventional analytical techniques, such as microscopic determination and scanning electron microscope (SEM).
- the preferred particle size diameter of the aluminosilicate is from about 0.1 micron to about 10 microns, more preferably from about 0.5 microns to about 9 microns. Most preferably, the particle size diameter is from about 1 microns to about 8 microns.
- the aluminosilicate ion exchange material has the formula Na z [(AlO 2 )z (SiO 2 )y]xH 2 O wherein z and y are integers of at least 6, the molar ratio of z to y is from about 1 to about 5 and x is from about 10 to about 264. More preferably, the aluminosilicate has the formula
- aluminosilicates are available commercially, for example under designations Zeolite A, Zeolite B and Zeolite X.
- Naturally-occurring or synthetically derived aluminosilicate ion exchange materials suitable for use herein can be made as described in Krummel et al, U.S. Patent No. 3,985,669, the disclosure of which is incorporated herein by reference.
- the aluminosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 mg equivalent of CaCO3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaCO3 hardness/gram. Additionally, the instant aluminosilicate ion exchange materials are still further characterized by their calcium ion exchange rate which is at least about 2 grains Ca ⁇ H 7gallon/minute/-gram/gallon, and more preferably in a range from about 2 grains Ca "H 7gallon/minute/-gram/gallon to about 6 grains Ca "H" /gallon/minute/-gram/gallon.
- An especially preferred set of dry detergent material is selected from the group consisting of aluminosilicates, crystalline layered silicates, sodium carbonate and mixtures thereof.
- the starting dry detergent material in the present process can include additional detergent ingredients and/or, any number of additional ingredients can be incorporated in the detergent composition during subsequent steps of the present process.
- adjunct ingredients include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressers, anti-tarnish and anti-corrosion agents, soil suspending agents, soil release agents, germicides, pH adjusting agents, non-builder alkalinity sources, chelating agents, smectite clays, enzymes, enzyme-stabilizing agents and perfumes. See U.S. Patent 3,936,537, issued February 3, 1976 to Baskerville, Jr. et al., incorporated herein by reference.
- Other builders can be generally selected from the various water-soluble, alkali metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, borates, polyhydroxy sulfonates, polyacetates, carboxylates, and polycarboxylates.
- alkali metal especially sodium, salts of the above.
- Preferred for use herein are the phosphates, carbonates, C ⁇ o-18 f "at ty cids, polycarboxylates, and mixtures thereof. More preferred are sodium tripolyphosphate, tetrasodium pyrophosphate, citrate, tartrate mono- and di-succinates, and mixtures thereof (see below).
- crystalline layered sodium silicates exhibit a clearly increased calcium and magnesium ion exchange capacity.
- the layered sodium silicates prefer magnesium ions over calcium ions, a feature necessary to insure that substantially all of the "hardness" is removed from the wash water.
- These crystalline layered sodium silicates are generally more expensive than amorphous silicates as well as other builders. Accordingly, in order to provide an economically feasible laundry detergent, the proportion of crystalline layered sodium silicates used must be determined judiciously.
- the crystalline layered sodium silicates suitable for use herein preferably have the formula
- the crystalline layered sodium silicate has the formula
- NaMSi O5.yH O wherein M is sodium or hydrogen, and y is from about 0 to about 20.
- inorganic phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of from about 6 to 21, and orthophosphates.
- polyphosphonate builders are the sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethane 1-hydroxy-l, 1-diphosphonic acid and the sodium and potassium salts of ethane, 1, 1,2-triphos- phonic acid.
- Other phosphorus builder compounds are disclosed in U.S. Patents 3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176 and 3,400, 148, all of which are incorporated herein by reference.
- nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of SiO- to alkali metal oxide of from about 0.5 to about 4.0, preferably from about 1.0 to about 2.4.
- Water-soluble, nonphosphorus organic builders useful herein include the various alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates.
- polyacetate and polycarboxylate builders are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylene diamine tetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid, mellitic acid, benzene polycarboxylic acids, and citric acid.
- Polymeric polycarboxylate builders are set forth in U.S. Patent 3,308,067, Diehl, issued March 7, 1967, the disclosure of which is incorporated herein by reference.
- Such materials include the water-soluble salts of homo- and copolymers of aliphatic carboxylic acids such as maleic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylene malonic acid.
- Some of these materials are useful as the water-soluble anionic polymer as hereinafter described, but only if in intimate admixture with the non-soap anionic surfactant.
- polyacetal carboxylates for use herein are the polyacetal carboxylates described in U.S. Patent 4, 144,226, issued March 13, 1979 to Crutchfield et al, and U.S. Patent 4,246,495, issued March 27, 1979 to Crutchfield et al, both of which are incorporated herein by reference.
- These polyacetal carboxylates can be prepared by bringing together under polymerization conditions an ester of glyoxylic acid and a polymerization initiator. The resulting polyacetal carboxylate ester is then attached to chemically stable end groups to stabilize the polyacetal carboxylate against rapid depolymerization in alkaline solution, converted to the corresponding salt, and added to a detergent composition.
- Particularly preferred polycarboxylate builders are the ether carboxylate builder compositions comprising a combination of tartrate monosuccinate and tartrate disuccinate described in U.S. Patent 4,663,071, Bush et al., issued May 5, 1987, the disclosure of which is incorporated herein by reference.
- Bleaching agents and activators are described in U.S. Patent 4,412,934, Chung et al., issued November 1, 1983, and in U.S. Patent 4,483,781, Hartman, issued November 20, 1984, both of which are incorporated herein by reference.
- Chelating agents are also described in U.S. Patent 4,663,071, Bush et al., from Column 17, line 54 through Column 18, line 68, incorporated herein by reference.
- Suds modifiers are also optional ingredients and are described in U.S. Patents 3,933,672, issued January 20, 1976 to Bartoletta et al., and 4,136,045, issued January 23, 1979 to Gault et al., both inco ⁇ orated herein by reference.
- Suitable smectite clays for use herein are described in U.S. Patent 4,762,645, Tucker et al, issued August 9, 1988, Column 6, line 3 through Column 7, line 24, inco ⁇ orated herein by reference.
- Suitable additional detergency builders for use herein are enumerated in the Baskerville patent, Column 13, line 54 through Column 16, line 16, and in U.S. Patent 4,663,071, Bush et al, issued May 5, 1987, both inco ⁇ orated herein by reference.
- a low density agglomerated detergent composition is prepared using a lab tilt-a-pin (commercially available from Processall, Inc.) mixer.
- the mixer is first charged with a mixture of powders, namely sodium carbonate (mean particle size of 5-40 microns made via Air Classifier Mill), light density, granular sodium tripolyphosphate (commercially supplied by FMC Co ⁇ . and referenced herein as "STPP”)), zeolite type A (commercially supplied by Ethyl Co ⁇ .
- Example IV did not use this or any fumed silica material.
- a surfactant paste containing sodium linear alkylbenzene sulfonate (“LAS” as referenced herein) surfactant (75% by weight) and the balance water is then added on top of the powder mixture while the mixer is operated for about 15 seconds at 700 ⁇ m until discrete granules are formed in the mixer.
- the composition of the agglomerates formed are set forth below in Table I.
- the resulting agglomerates of Examples I, II and II have a bulk density below 500 g/L, all of which are made by a process involving silica and within the scope of the process invention.
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Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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AT97934907T ATE242308T1 (de) | 1996-07-26 | 1997-07-16 | Herstellung von kieselsäure enthaltende waschmittelagglomerate mit niedriger dichte |
DE69722627T DE69722627T2 (de) | 1996-07-26 | 1997-07-16 | Herstellung von kieselsäure enthaltende waschmittelagglomerate mit niedriger dichte |
AU37964/97A AU3796497A (en) | 1996-07-26 | 1997-07-16 | Preparation of low ldensity detergent agglomerates containing silica |
EP97934907A EP0915958B1 (en) | 1996-07-26 | 1997-07-16 | PREPARATION OF LOW lDENSITY DETERGENT AGGLOMERATES CONTAINING SILICA |
BR9710558A BR9710558A (pt) | 1996-07-26 | 1997-07-16 | Prepara-Æo de aglomerados de detergente de baixa densidade contendo silica |
Applications Claiming Priority (2)
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US2281696P | 1996-07-26 | 1996-07-26 | |
US60/022,816 | 1996-07-26 |
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PCT/US1997/011985 WO1998004669A1 (en) | 1996-07-26 | 1997-07-16 | PREPARATION OF LOW lDENSITY DETERGENT AGGLOMERATES CONTAINING SILICA |
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CN (1) | CN1116402C (pt) |
AR (1) | AR008785A1 (pt) |
AT (1) | ATE242308T1 (pt) |
AU (1) | AU3796497A (pt) |
BR (1) | BR9710558A (pt) |
DE (1) | DE69722627T2 (pt) |
ES (1) | ES2196352T3 (pt) |
ID (1) | ID19363A (pt) |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0510746A2 (en) * | 1991-04-12 | 1992-10-28 | The Procter & Gamble Company | Process for preparing condensed detergent granules |
JPH07179898A (ja) * | 1993-12-22 | 1995-07-18 | Lion Corp | 高嵩密度粒状洗剤組成物の製造方法 |
US5576285A (en) * | 1995-10-04 | 1996-11-19 | The Procter & Gamble Company | Process for making a low density detergent composition by agglomeration with an inorganic double salt |
WO1997010321A1 (en) * | 1995-09-12 | 1997-03-20 | The Procter & Gamble Company | Compositions comprising hydrophilic silica particulates |
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BR9205892A (pt) * | 1991-04-12 | 1994-09-27 | Procter & Gamble | Aglomeraçao de pastas altamente ativas para formargranulos de tensoativos uteis em composiçoes detergentes. |
-
1997
- 1997-07-16 AU AU37964/97A patent/AU3796497A/en not_active Abandoned
- 1997-07-16 BR BR9710558A patent/BR9710558A/pt not_active IP Right Cessation
- 1997-07-16 ES ES97934907T patent/ES2196352T3/es not_active Expired - Lifetime
- 1997-07-16 CN CN97197976A patent/CN1116402C/zh not_active Expired - Fee Related
- 1997-07-16 WO PCT/US1997/011985 patent/WO1998004669A1/en active IP Right Grant
- 1997-07-16 DE DE69722627T patent/DE69722627T2/de not_active Expired - Fee Related
- 1997-07-16 EP EP97934907A patent/EP0915958B1/en not_active Expired - Lifetime
- 1997-07-16 AT AT97934907T patent/ATE242308T1/de not_active IP Right Cessation
- 1997-07-24 AR ARP970103365A patent/AR008785A1/es unknown
- 1997-07-24 ZA ZA9706618A patent/ZA976618B/xx unknown
- 1997-07-28 ID IDP972620A patent/ID19363A/id unknown
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0510746A2 (en) * | 1991-04-12 | 1992-10-28 | The Procter & Gamble Company | Process for preparing condensed detergent granules |
JPH07179898A (ja) * | 1993-12-22 | 1995-07-18 | Lion Corp | 高嵩密度粒状洗剤組成物の製造方法 |
WO1997010321A1 (en) * | 1995-09-12 | 1997-03-20 | The Procter & Gamble Company | Compositions comprising hydrophilic silica particulates |
US5576285A (en) * | 1995-10-04 | 1996-11-19 | The Procter & Gamble Company | Process for making a low density detergent composition by agglomeration with an inorganic double salt |
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DATABASE WPI Week 9537, Derwent World Patents Index; AN 95-281206, XP002050465 * |
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ZA976618B (en) | 1998-02-10 |
CN1116402C (zh) | 2003-07-30 |
ATE242308T1 (de) | 2003-06-15 |
CN1230982A (zh) | 1999-10-06 |
ID19363A (id) | 1998-07-02 |
EP0915958B1 (en) | 2003-06-04 |
DE69722627T2 (de) | 2004-04-29 |
DE69722627D1 (de) | 2003-07-10 |
AR008785A1 (es) | 2000-02-23 |
AU3796497A (en) | 1998-02-20 |
BR9710558A (pt) | 1999-08-17 |
EP0915958A1 (en) | 1999-05-19 |
ES2196352T3 (es) | 2003-12-16 |
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