CA2295941C - Process for making a low density detergent composition by controlling nozzle height in a fluid bed dryer - Google Patents
Process for making a low density detergent composition by controlling nozzle height in a fluid bed dryer Download PDFInfo
- Publication number
- CA2295941C CA2295941C CA002295941A CA2295941A CA2295941C CA 2295941 C CA2295941 C CA 2295941C CA 002295941 A CA002295941 A CA 002295941A CA 2295941 A CA2295941 A CA 2295941A CA 2295941 C CA2295941 C CA 2295941C
- Authority
- CA
- Canada
- Prior art keywords
- agglomerates
- detergent
- fluid bed
- bed dryer
- built
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000003599 detergent Substances 0.000 title claims abstract description 114
- 238000000034 method Methods 0.000 title claims abstract description 81
- 230000008569 process Effects 0.000 title claims abstract description 77
- 239000012530 fluid Substances 0.000 title claims abstract description 36
- 239000000203 mixture Substances 0.000 title claims description 34
- 239000004094 surface-active agent Substances 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 31
- 239000011230 binding agent Substances 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 18
- -1 alkylbenzene sulfonate Chemical class 0.000 claims description 17
- 239000004115 Sodium Silicate Substances 0.000 claims description 16
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 9
- 230000004907 flux Effects 0.000 claims description 6
- 239000002245 particle Substances 0.000 description 26
- 229910000323 aluminium silicate Inorganic materials 0.000 description 18
- 239000004615 ingredient Substances 0.000 description 18
- 239000008187 granular material Substances 0.000 description 17
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 16
- 238000005342 ion exchange Methods 0.000 description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 14
- 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
- 239000003945 anionic surfactant Substances 0.000 description 10
- 229910052708 sodium Inorganic materials 0.000 description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 description 8
- 235000019351 sodium silicates Nutrition 0.000 description 7
- 235000019832 sodium triphosphate Nutrition 0.000 description 7
- 238000001694 spray drying Methods 0.000 description 6
- 229910001424 calcium ion Inorganic materials 0.000 description 5
- 150000007942 carboxylates Chemical class 0.000 description 5
- 229920005646 polycarboxylate Polymers 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 150000004760 silicates Chemical class 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical group [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 229930182556 Polyacetal Natural products 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000002736 nonionic surfactant Substances 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 229920006324 polyoxymethylene Polymers 0.000 description 4
- 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
- 101710194948 Protein phosphatase PhpP Proteins 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 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
- 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
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 159000000001 potassium salts Chemical class 0.000 description 3
- 238000012216 screening Methods 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
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 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
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 150000004996 alkyl benzenes Chemical class 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 238000001035 drying Methods 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
- 238000011031 large-scale manufacturing process 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
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229910021647 smectite Inorganic materials 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 150000003871 sulfonates Chemical class 0.000 description 2
- 239000010457 zeolite Substances 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
- 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
- 201000004002 Aromatase excess syndrome Diseases 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-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
- 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
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical class CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical class OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-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
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 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
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-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
- 229940091181 aconitic acid Drugs 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 150000008051 alkyl sulfates Chemical class 0.000 description 1
- 150000001412 amines Chemical class 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
- 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
- 238000006243 chemical reaction Methods 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
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 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
- 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
- 229960001484 edetic acid Drugs 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
- UZABCLFSICXBCM-UHFFFAOYSA-N ethoxy hydrogen sulfate Chemical class CCOOS(O)(=O)=O UZABCLFSICXBCM-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000000945 filler Substances 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
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 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
- 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
- 239000003002 pH adjusting agent Substances 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
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000002459 porosimetry 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
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000000375 suspending agent Substances 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
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-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
- 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
- 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
- C11D11/0088—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 the liquefied ingredients being sprayed or adsorbed onto solid particles
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Detergent Compositions (AREA)
Abstract
A process for preparing low density detergent agglomerates having a density in a range from about 300 g/l to about 550 g/l is provided. The process involve s the steps of: (a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates; (b) mixing the agglomerates in a second high speed mixe r to obtain built-up agglomerates; and (c) feeding the built-up agglomerates into a fluid bed dryer in which a binder is sprayed via a nozzle having a height of from about 25 cm to about 60 cm from the distributor plate of the fluid bed dryer such that the built-up agglomerate are dried and agglomerate d to form the desired low detergent agglomerates.
Description
PROCESS FOR MAKING A LOW DENSITY DETERGENT COMPOSITIOV BY
CONTROLLING NOZZLE HEIGHT IN A FLUID BED DRYER
FIELD OF THE INVENTION
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 or liquid acid precursor of anionic surfactant and dry starting detergent material sequentially into two high speed mixers followed by a fluid bed dryer which has an optimally selected nozzle height for spraying on a binder. 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.
BACKGROUND OF THE INVENTION
Recently, there has been considerable interest within the detergent industry for laundry detergents which are "compact" and therefore, have low dosage volumes.
To facilitate production of these so-called low dosage detergents, many attempts have been made to produce high bulk density detergents, for example with a density of 600 g/1 or higher. The low dosage detergents are currently in high demand as they conserve resources and can be sold in small packages which are more convenient for consumers.
However, the extent to which modern detergent products need to be "compact" in nature remains unsettled. In fact, many consumers, especially in developing countries, continue to prefer a higher dosage levels in their respective laundering operations. Consequently, there is a need in the art of producing modern detergent compositions for flexibility in the ultimate density of the final composition.
Generally, there are two primary types of processes by which detergent granules or powders can be prepared. The first type of process involves spray-drying an aqueous detergent slurry in a spray-drying tower to produce highly porous detergent granules. In the second type of process, the various detergent components are dry mixed after which they are agglomerated with a binder such as a nonionic or anionic surfactant.
In both processes, the most important factors which govern the density of the resulting detergent granules are the density, porosity and surface area, shape of the various starting materials and their respective chemical composition. These parameters, however, can only be varied within a limited range. Thus, flexibility in the substantial bulk density can only be achieved by additional processing steps which lead to lower density of the detergent granules.
There have been many attempts in the art for providing processes which increase the density of detergent granules or powders. Particular attention has been eiven to densification of spray-dried granules by post tower treatment. For example, one attempt involves a batch process in which spray-dried or granulated detergent powders containing sodium tripolyphosphate and sodium sulfate are densified and spheronized in a Marumerizer~. This apparatus comprises a substantially horizontal, roughened, rotatable table positioned within and at the base of a substantially vertical, smooth walled cylinder.
This process, however, is essentially a batch process and is therefore less suitable for the large scale production of detergent powders. More recently, other attempts have been made to provide continuous processes for increasing the density of "post-tower" or spray dried detergent granules. Typically, such processes require a first apparatus which pulverizes or grinds the granules and a second apparatus which increases the density of the pulverized granules by agglomeration. While these processes achieve the desired increase in density by treating or densifying "post tower" or spray dried granules, they do not provide a process which has the flexibility of providing lower density granules.
Moreover, all of the aforementioned processes are directed primarily for densifying or otherwise processing spray dried granules. Currently, the relative amounts and types of materials subjected to spray drying processes in the production of detergent granules has been limited. For example, it has been difficult to attain high levels of surfactant in the resulting detergent composition, a feature which facilitates production of detergents in a more efficient manner. Thus, it would be desirable to have a process by which detergent compositions can be produced without having the limitations imposed by conventional spray drying techniques.
To that end, the art is also replete with disclosures of processes which entail agglomerating detergent compositions. For example, attempts have been made to agglomerate detergent builders by mixing zeolite and/or layered silicates in a mixer to form free flowing agglomerates. While such attempts suggest that their process can be used to produce detergent agglomerates, they do not provide a mechanism by which conventional starting detergent materials in the form of surfactant pastes or precursors thereof, liquids and dry materials can be effectively agglomerated into crisp, free flowing detergent agglomerates having low densities rather than high densities. In the past, attempts at producing such low density agglomerates involves a nonconventional detergent ingredient which is typically expensive, thereby adding to the cost of the detergent product. One such example of this involves a process of agglomerating with inorganic double salts such as Burkeite to produce the desired low density agglomerates.
Accordingly, there remains a need in the art to have a process for producing a low density detergent composition directly from starting detergent ingredients without the need for relatively expensive specialty ingredients. Also, there remains a need for such a process which is more efficient, flexible and economical to faciiitate large-scaie production of detergents of low as well as high dosage levels.
BACKGROUND ART
The following references are directed to densifying spray-dried granules:
Appel et al. U.S. Patent No. 5,133,924 (Lever); Bortolotti et al, U.S. Patent No.
5,160,657 (Lever);
Johnson et al, British patent No. 1,517,713 (Unilever); and Curtis, European Patent Application 451,894. The following references are directed to producing detergents by agglomeration: Beerse et at, U.S. Patent No. 5,108,646 (Procter & Gamble);
Capeci et al, U.S. Patent No. 5.366,652 (Procter & Gamble); Hollingsworth et al, European Patent Application 351,937 (Unilever); and Swatting et al, U.S. Patent No. 5,205,958.
The following references are directed to inorganic double salts: Evans et al, U.S.
Patent No.
I O 4,820,441 (Lever); Evans et al, U.S. Patent No. 4,818,424 (Lever);
Atkirison et al, U.S.
Patent No. 4,900,466 (Lever); France et al, U.S. Patent No. 5,576,285 (Procter & Gamble);
and Dhalewadika et al, PCT WO 96/04359 (Unilever).
SUMMARY OF THE INVENTION
The present invention meets the aforementioned needs in the art by providing a 15 process which produces a low density (below about 600 g/1) detergent composition directly from a surfactant paste and dry starting detergent ingredients. In essence, the process involves agglomerating the starting detergent ingredients in a high speed mixer followed by a second high speed mixer. Thereafter, the agglomerates formed in the high speed mixers are agglomerated and dried in a fluid bed dryer in which a liquid binder is sprayed onto the 20 agglomerates from one or more nozzles at a selected height from the distribution plate of the fluid bed dryer. 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 25 towers which typically emit particulates and volatile organic compounds into the atmosphere.
As used herein, the term "agglomerates" refers to particles formed by agglomerating detergent granules or particles which typically have a smaller median particle size than the formed agglomerates. By "median particle size", it is meant the 30 particle size diameter value above which SO% of the particles have a larger particle size and below which 50% of particles have a smaller particle size. All percentages used herein are expressed as "percent-by-weight" on an anhydrous basis unless indicated otherwise.
In accordance with one aspect of the invention, a process for preparing low density detergent agglomerates is provided. The process comprises the steps of: (a) agglomerating 35 a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates; (b) mixing the agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding the built-up agglomerates into a fluid bed dryer in which a binder is sprayed via a nozzle having a height of from about 2~
cm to about 60 cm from the distributor plate of the fluid bed dryer such that the built-up agglomerates are dried and agglomerated to form the low density detergent agglomerates having a density in a range from about 300 g/1 to about 550 g/1.
In accordance with another aspect of the invention, another process for preparing low density detergent agglomerates is provided. The process comprises the steps of: (a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates; (b) mixing the agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding the built-up agglomerates into a fluid bed dryer in which sodium silicate is sprayed via a nozzle having a height of from about 40 cm to about GO cm from the distributor plate of the fluid bed dryer such that the built-up agglomerates are dried and agglomerated to form the low density detergent agglomerates having a density in a range from about 300 g/1 to about 550 g,~l.
The detergent products made in accordance with any of the process embodiments described herein are also provided.
Accordingly, it is an object of the invention to provide a process for producing a low density detergent composition directly from starting detergent ingredients which does not include relatively expensive specialty ingredients. It is also an object of the invention to provide such a process which is more efficient, flexible and economical so as to facilitate large-scale production of detergents of low as well as high dosage levels.
These and other objects, features and attendant advantages of the present invention will become apparent to those skilled in the art from a reading of the following detailed description of the preferred embodiment and the appended claims.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention is directed to a process in which low density agglomerates are produced by a three step process, the last of which involves a fluid bed dryer containing one or more nozzles positioned at a selected height from the distribution plate of the dryer.
In this way, the process forms free flowing, low density detergent agglomerates which can be used alone as the detergent product or as an admixture with conventional spray-dried detergent granules and/or high density detergent agglomerates in a final commercial detergent product. It should be understood that the process described herein can be operated cpntinuously or in a batch mode depending upon the particularly desired application. One major advantage of the present process is that it utilizes equipment which can be operated differently from the present process parameters to obtain high density detergent compositions. Thus, a single large-scale commercial detergent manufacturing facility can be built to produce high or low density detergent compositions depending upon the local consumer demand and its inevitable fluctuations between compact and non-compact detergent products.
Process In the first step of the process. a detergent surfactant paste or precursor thereof as set forth in more detail hereinafter and dry starting detergent material is inputted and agglomerated in a high speed mixer. Unlike previous processes in this area, the dry starting material can include only those relatively inexpensive detergent materials typically used in modern granular detergent products. Such ingredients, include but are not limited to, builders, fillers, dry surfactants, and flow aides. Preferably, the builder includes aluminosilicates, crystalline layered silicates, phosphates, carbonates and mixtures thereof which is the essential dry starting detergent ingredient within the scope of the current process. Relatively expensive materials such as Burkeite (Na2S04~Na2C03) and the various silicas are not necessary to achieve the desired low density agglomerates produced by the process. Rather, by selecting the binder and nozzle height through which the binder is sprayed onto the agglomerates in the fluid bed dryer as described in more detail hereinafter, the present process achieves the desired low density. Further, it is preferable to include from 1 % to about 40% by weight of undersized detergent particles or "fines" in the first step of the process. This can be conveniently accomplished by screening the detergent particles formed subsequent to the fluid bed dryer to a median particle size range of from about 10 microns to about 150 microns and feeding these "fines" back into the first high speed mixer.
The high speed mixer can be any one of a variety of commercially available mixers TM
such as a Lodige CB 30 mixer or similar brand mixer. These types of mixers essentially consist of a horizontal, hollow static cylinder having a centrally mounted rotating shaft around which several shovel and rod-shaped blades are attached which have a tip speed of from about 5 m/s to about 30 m/s, more preferably from about 6 m/s to about 26 mls.
Preferably, the shaft rotates at a speed of from about 100 rpm to about 2500 rpm, more preferably from about 300 rpm to about 1600 rpm. Preferably, the mean residence time of the detergent ingredients in the high speed mixer is preferably in range from about 2 seconds to about 45 seconds, and most preferably from about 5 seconds to about seconds. This mean residence time is conveniently measured by dividing the weight of the mixer at steady state by throughput (kg/hr) flow. Another suitable mixer is any one of the TM TM
various Flexomix models available from Schugi (Netherlands) which are vertically positioned high speed mixers. This type of mixer is preferably operated at a Froude Index of from about 13 to about 32. See U.S. Patent 5,149,455 to Jacobs et al (issued September 22, 1992) for a detailed discussion of this well-known Froude Index which is a dimensionless number that can be optimally selected by those skilled in the art.
In a prefen;ed embodiment of the process invention, a liquid acid precursor of an anionic surfactant is inputted with the dry starting detergent material which at least includes a neutralizing agent such as sodium carbonate. The preferred liquid acid surfactant precursor is Cl 1-18 linear alkylbenzene sulfonate surfactant ("HLAS"), although any acid precursor of an anionic surfactant may be used in the process. A more preferred embodiment involves feeding a liquid acid precursor of C 12_ 14 linear alkylbenzene sulfonate surfactant with a C10-18 alkyl ethoxylated sulfate ("AS") surfactant into the first high speed mixer, preferably in a weight ratio of from about 5:1 to about 1:~, and most preferably, in a range of from about 1:1 to about 3:1 (HLAS:AS). The result of such mixing is a "dry neutralization" reaction between the HLAS and the sodium carbonate embodied in the dry starting detergent material, all of which forms agglomerates. It is preferable to add the HLAS before the addition of other surfactants such as AS
or alkyl ethoxylate sulfate ("AES") surfactants so as to insure optimal mixing and neutralization of the HLAS in the first high speed mixer. In the second step of the process, the detergent agglomerates formed in the first step are inputted into a second high speed mixer which can be the same piece of equipment as used in the first step or a differern type 1 S of high speed mixer. For example, a Lodige CB mixer can be used in the first step while a Schugi mixer is used in the second step. in this second process step, the agglomerates are mixed and built-up further in a controlled fashion. In this step, a sufficient amount of binder can be inputted to facilitate agglomeration build-up in the mixer.
Typical binders include liquid sodium silicate, a liquid acid precursor of an anionic surfactant such as HLAS, nonionic surfactant, polyethylene glycol or mixtures thereof.
In the next step of the process, the built-up agglomerates are inputted into a fluid bed dryer in which the agglomerates are dried and agglomerated to a median particle size of from about 300 microns to about 700 microns, more preferably from about 325 microns to about 450 microns. The density of the agglomerates formed is from about 300 g/1 to about 550 g/1, more preferably from about 350 g/1 to about 500 gll, and even more preferably from about 400 g/1 to about 480 g/1. All of these densities are generally below that of typical detergent compositions formed of dense agglomerates or most typical spray-dried granules.
A binder as described previously is preferably added during this step to enhance formation of the desired agglomerates. In this regard, a particularly preferred binder is liquid sodium silicate in an amount of from about 0.1% to about 20% by weight of the final low density composition. The nozzle height through which the binder is added is preferably from about 25 cm to about 60 cm, more preferably from about 30 cm to about b0 cm, most preferably from about 40 cm to about 60 cm, and even more preferably at 40 cm, from the distribution plate of the fluid bed dryer. Preferably all of the nozzles used in the fluid bed drying apparatus have such a height arrangement. Unexpectedly, it has been found that by selecting the nozzle height to be within the aforementioned ranges, superior low density agglomerates are produced in the process from both a low density and free flowability standpoint.
Additionally. the benefits of the process in this regard can be enhanced by maintaining the spray-on flux of the binder in the fluid bed to be from about 0.02 kQ. cm2/hr to about 0.06 kg/cm2/hr, more preferably from about 0.04 kg/cm2/hr to about 0.05 ' kg/cm2/hr. Preferably, the air inlet temperature in the fluid bed dryer is from about 100°C
to about 200°C, more preferably from about 110°C to about 130°C. Also, the unfluidized bed height in fluid bed dryer is preferably from about 5 cm to about 20 cm. It has also been found that the process benefits can be enhanced by maintaining the fluidized air flux in the fluid bed dryer is from about 0.6 kg/m2/s to about 0.8 kg/m2/s. It has also been found beneficial to add the binder simultaneously at more than one location in one or more of the steps of the process. For example, the liquid silicate can be added at two locations in the fluid bed dryer, e.g., at or near the inlet port and at or near the exit port.
Also, the median binder droplet diameter is from about 20 microns to about 150 microns, a parameter which enhances formation of the desired built-up agglomerates. Further in this regard, the ratio of the median binder droplet diameter to built-up agglomerate (exiting the second high speed mixer) particle diameter is preferably from about 0.1 to about 0.6.
Optionally, the process may involve adding the binder to both the second high speed mixer as well as the fluid bed dryer. It has also been found beneficial to add the binder simultaneously at more than one location in one or more of the steps of the process.
For example, the liquid silicate can be added at two locations in the fluid bed dryer, e.g., at or near the inlet port and at or near the exit port. As with the first and second steps of the process, the agglomerates are built-up from smaller sizes to large sized particles having a high degree of intraparticie porosity. The degree of intraparticle porosity is preferably from about 20% to about 40%, and most preferably from about 25% to about 35%. The intraparticle porosity can be conveniently measured by standard mercury porosimetry testing.
Other 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 inciude conditioning of the detergent agglomerates by subjecting the agglomerates to additional drying and/or cooling by way of apparatus discussed previously.
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. For example, 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.
Detergent Surfactant Paste or Precursor The liquid acid precursor of anionic surfactant is used in the first step of the process, and in optional embodiments, as a liquid binder in the second and,~or third essential steps of the process. This liquid acid precursor will typically have a viscosity measured at 30°C of from about 500 cps to about 5.000 cps. The liquid acid is a precursor for the anionic surfactants described in more detail hereinafter. A detergent surfactant paste can also be used in the process and is preferably in the form of an aqueous viscous paste, although other 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.' 1. Furthermore, 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. 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. Of the surfactants, anionics and nonionics are preferred and anionics are most preferred.
Nonlimiting examples of the preferred anionic surfactants useful in the surfactant paste, or from which the liquid acid precursor described herein derives, include the conventional C11-Clg alkyl benzene sulfonates ("LAS"), primary, branched-chain and random C10-C20 alkyl sulfates ("AS"), the C10-Clg secondary (2,3) alkyl sulfates of the formula CH3(CH2)x(CHOS03 M+) CH3 and CH3 (CH2)y(CHOS03 M+) CH2CH3 where x and (y + 1 ) are integers of at least about 7, preferably at least about 9, and M is a 510 water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, and the C10-Clg alkyl alkoxy sulfates ("AEXS"; especially EO 1-7 ethoxy sulfates).
Optionally, other exemplary surfactants useful in the paste of the invention include and C 10-C 1 g alkyl alkoxy carboxylates (especially the EO 1-S
ethoxycarboxylates), the C10-18 glycerol ethers, the C10-C1 g alkyl polyglycosides and their corresponding sulfated polyglycosides, and C12-Clg alpha-sulfonated fatty acid esters. If desired, the conventional nonionic and amphoteric surfactants such as the C 12-C 1 g alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and C6-C12 alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxyipropoxy), C 1 ~-C I g betaines and sulfobetaines ("sultaines"), CIO-Clg amine oxides, and the like, can also be included in the overall compositions. The C l p-C 1 g N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C12-C1g N-methylglucamides. See WO
9,206,154.
Other sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C 10-C 1 g N-(3-methoxypropyl) glucamide. The N-propyl through N-hexyl C 12-C 1 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 l0-C 16 soaps may be used.
Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are listed in standard texts.
Dry Detergent Material The starting dry detergent material of the present process preferably comprises a builder and other standard detergent ingredients such as sodium carbonate, especially when a liquid acid precursor of a surfactant is used as it is needed as a neutralizing agent in the I S first step of the process. Thus, preferable starting dry detergent material includes sodium carbonate and a phosphate or an aluminosilicate builder which is referenced as an aluminosilicate ion exchange material. A preferred builder is selected from the group consisting of aluminosilicates, crystalline layered silicates, phosphates, carbonates and mixtures thereof. Preferred phosphate builders include sodium tripolyphosphate, tetrasodium pyrophosphate and mixtwes thereof. Additional specific examples of inorganic phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of from about 6 to 21, and orthophosphates. Examples of polyphosphonate builders are the sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethane 1-hydroxy-1, 1-diphosphonic acid and the sodium and potassium salts of ethane, 1,1,2-triphosphonic 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.
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. In that regard, 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) .
1~
Preferably, the aiuminosilicate 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. Additionally, 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 panicle size diameters which optimize their effectiveness as detergent builders. The term "particle size diameter"
as used herein represents the average particle size diameter of a given aluminosilicate ion exchange material as determined by conventional analytical techniques, such as microscopic l0 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.
Preferably, the aluminosilicate ion exchange material has the formula Naz[(A102)z.( Si02)y]xH20 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 Na 12~~A102) 12~(Si02) 12]~20 wherein x is from about 20 to about 30, preferably about 27. These preferred aluminosilicates are available commercially, for example under designations Zeolite A, Zeolite B and Zeolite X. Alternatively, 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 aluminosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 mg equivalent of CaC03 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaC03 hardness/gram. Additionally, the instant aluminosilicate ion exchange materials are still further character7zed by their calcium ion exchange rate which is at least about 2 grains Ca'+'r/gallon/minute/-gram/gallon, and more preferably in a range from about 2 grains Ca'~/gallon/minute/-gram/gallon to about 6 grains Ca~/gallon/minute/-gram/gallon .
Adiunct Detereent Intredients The starting dry detergent material in the present process can include additional detergent ingredients andlor, any number of additional ingredients can be incorporated in the detergent composition during subsequent steps of the present process.
These adjunct ingredients include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressors, anti-tarnish and anticorrosion 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 _ 3,936.37, issued February 3, 1976 to Baskerville, Jr. et ai .
Other builders can be generally selected from the various borates, polyhydroxy sulfonates, polyacetates, carboxylates, citrates, tarnate mono- and di-succinates, and mixtures thereof. Preferred are the alkali metal, especially sodium, salts of the above. In comparison with amorphous sodium silicates, crystalline layered sodium silicates exhibit a clearly increased calcium and magnesium ion exchange capacity. In addition, 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, however, are generally more expensive than amorphous silicates 1 S 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 ~ NaMSix02x+l.yH20 wherein M is sodium or hydrogen, x is from about 1.9 to about 4 and y is from about 0 to about 20. More preferably, the crystalline layered sodium silicate has the formula NaMSi205.yH20 wherein M is sodium or hydrogen, and y is from about 0 to about 20. These and other crystalline layered sodium silicates are discussed in Corkill et al, U.S.
Patent No.
4,605,509.
Examples of nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of Si02 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.
Examples of 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. Such materials include the water-soluble salts of homo- and copolymers of aliphatic carboxylic l~
acids such as malefic acid, itacontc 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.
Other suitable polycarboxylates 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. 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, convened to the corresponding salt, and added to a detergent composition. Particularly prefer ed polycarboxylate builders are the ether carboxylate builder compositions comprising a combination of tarnate monosuccinate and tarnate disuccinate described in U.S. Patent 4,663,071, Bush et al., issued May 5, 1987.
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. 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. 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.
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~
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.
In order to make the present invention more readily understood, reference is made to the following example, which is intended to be illustrative only and not intended to be limiting in scope.
EXAMPLE
This Example illustrates the process invention in which a low density agglomerated detergent composition is prepared. A Lodige CB 30 high speed mixer is charged with a mixture of powders, namely sodium carbonate (median particle size 15 microns) and sodium tripolyphosphate ("STPP") with a median particle size of 25 microns.
A liquid acid precursor of sodium alkylbenzene sulfonate surfactant (C 12H25-H or "HLAS" as noted below) and a 70% active aqueous C 10_I g alkyl ethoxylated sulfate surfactant (E0 = 3, "AES") paste are also inputted into the Lodige CB 30 mixer, wherein the HLAS is added first. The mixer is operated at 1600 rpm and the sodium carbonate, STPP, HLAS and AES are formed into agglomerates having a median particle size of about 110 microns after a mean residence time in the Lodige CB 30 mixer of about 5 seconds. The agglomerates are then fed to a Schugi (Model # FX160) high speed mixer which is operated at 2800 rpms with a mean residence time of about 2 seconds.
A HLAS
binder is inputted into the Schugi (Model # FX160) mixer during this step which results in built-up agglomerates having a median particle size of about 180 microns being formed.
Thereafter, the built-up agglomerates are passed through a four-zone fluid bed dryer which is operated at an air inlet temperature of about 125°C and a nozzle height of 40 cm from the distribution plate in the first and fourth zones of the fluid bed. The spray-on flux of the sodium silicate in 0.04 kg/cm2/hr, the unfluidized bed height is 10 cm, and the fluidized air flux is 0.6 kg/m2/s. In the amounts and particle size specified below, fines are also added to the Lodige CB 30 mixer. In the first and fourth zones of the fluid bed dryer, liquid sodium silicate is fed into the fluid bed dryer resulting in the finished detergent agglomerates having a density of about 485 g/1 and a median particle size of about 360 microns. Unexpectedly, the finished agglomerates have excellent physical properties in that they are free flowing as exhibited by their superior cake strength grades.
The composition of the agglomerates are given below in Table I.
TABLEI
(% weight) Component I
LAS (Na) 15.8 AES (E0 = 3) 4.7 Sodium carbonate 48.0 STPP 22.7 Sodium Silicate 5.5 Water 3.3 100.0 The agglomerates embody about 14% of fines (less than 150 microns) which are recycled from the fluid bed back into the Lodige CB 30 which enhances production of the agglomerates produced by the process.
~/ J
Having thus described the invention in detail, it will be clear to those skilled in the art that various changes may be made without departing from the scope of the invention and the invention is not to be considered limited to what is described in the specification.
CONTROLLING NOZZLE HEIGHT IN A FLUID BED DRYER
FIELD OF THE INVENTION
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 or liquid acid precursor of anionic surfactant and dry starting detergent material sequentially into two high speed mixers followed by a fluid bed dryer which has an optimally selected nozzle height for spraying on a binder. 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.
BACKGROUND OF THE INVENTION
Recently, there has been considerable interest within the detergent industry for laundry detergents which are "compact" and therefore, have low dosage volumes.
To facilitate production of these so-called low dosage detergents, many attempts have been made to produce high bulk density detergents, for example with a density of 600 g/1 or higher. The low dosage detergents are currently in high demand as they conserve resources and can be sold in small packages which are more convenient for consumers.
However, the extent to which modern detergent products need to be "compact" in nature remains unsettled. In fact, many consumers, especially in developing countries, continue to prefer a higher dosage levels in their respective laundering operations. Consequently, there is a need in the art of producing modern detergent compositions for flexibility in the ultimate density of the final composition.
Generally, there are two primary types of processes by which detergent granules or powders can be prepared. The first type of process involves spray-drying an aqueous detergent slurry in a spray-drying tower to produce highly porous detergent granules. In the second type of process, the various detergent components are dry mixed after which they are agglomerated with a binder such as a nonionic or anionic surfactant.
In both processes, the most important factors which govern the density of the resulting detergent granules are the density, porosity and surface area, shape of the various starting materials and their respective chemical composition. These parameters, however, can only be varied within a limited range. Thus, flexibility in the substantial bulk density can only be achieved by additional processing steps which lead to lower density of the detergent granules.
There have been many attempts in the art for providing processes which increase the density of detergent granules or powders. Particular attention has been eiven to densification of spray-dried granules by post tower treatment. For example, one attempt involves a batch process in which spray-dried or granulated detergent powders containing sodium tripolyphosphate and sodium sulfate are densified and spheronized in a Marumerizer~. This apparatus comprises a substantially horizontal, roughened, rotatable table positioned within and at the base of a substantially vertical, smooth walled cylinder.
This process, however, is essentially a batch process and is therefore less suitable for the large scale production of detergent powders. More recently, other attempts have been made to provide continuous processes for increasing the density of "post-tower" or spray dried detergent granules. Typically, such processes require a first apparatus which pulverizes or grinds the granules and a second apparatus which increases the density of the pulverized granules by agglomeration. While these processes achieve the desired increase in density by treating or densifying "post tower" or spray dried granules, they do not provide a process which has the flexibility of providing lower density granules.
Moreover, all of the aforementioned processes are directed primarily for densifying or otherwise processing spray dried granules. Currently, the relative amounts and types of materials subjected to spray drying processes in the production of detergent granules has been limited. For example, it has been difficult to attain high levels of surfactant in the resulting detergent composition, a feature which facilitates production of detergents in a more efficient manner. Thus, it would be desirable to have a process by which detergent compositions can be produced without having the limitations imposed by conventional spray drying techniques.
To that end, the art is also replete with disclosures of processes which entail agglomerating detergent compositions. For example, attempts have been made to agglomerate detergent builders by mixing zeolite and/or layered silicates in a mixer to form free flowing agglomerates. While such attempts suggest that their process can be used to produce detergent agglomerates, they do not provide a mechanism by which conventional starting detergent materials in the form of surfactant pastes or precursors thereof, liquids and dry materials can be effectively agglomerated into crisp, free flowing detergent agglomerates having low densities rather than high densities. In the past, attempts at producing such low density agglomerates involves a nonconventional detergent ingredient which is typically expensive, thereby adding to the cost of the detergent product. One such example of this involves a process of agglomerating with inorganic double salts such as Burkeite to produce the desired low density agglomerates.
Accordingly, there remains a need in the art to have a process for producing a low density detergent composition directly from starting detergent ingredients without the need for relatively expensive specialty ingredients. Also, there remains a need for such a process which is more efficient, flexible and economical to faciiitate large-scaie production of detergents of low as well as high dosage levels.
BACKGROUND ART
The following references are directed to densifying spray-dried granules:
Appel et al. U.S. Patent No. 5,133,924 (Lever); Bortolotti et al, U.S. Patent No.
5,160,657 (Lever);
Johnson et al, British patent No. 1,517,713 (Unilever); and Curtis, European Patent Application 451,894. The following references are directed to producing detergents by agglomeration: Beerse et at, U.S. Patent No. 5,108,646 (Procter & Gamble);
Capeci et al, U.S. Patent No. 5.366,652 (Procter & Gamble); Hollingsworth et al, European Patent Application 351,937 (Unilever); and Swatting et al, U.S. Patent No. 5,205,958.
The following references are directed to inorganic double salts: Evans et al, U.S.
Patent No.
I O 4,820,441 (Lever); Evans et al, U.S. Patent No. 4,818,424 (Lever);
Atkirison et al, U.S.
Patent No. 4,900,466 (Lever); France et al, U.S. Patent No. 5,576,285 (Procter & Gamble);
and Dhalewadika et al, PCT WO 96/04359 (Unilever).
SUMMARY OF THE INVENTION
The present invention meets the aforementioned needs in the art by providing a 15 process which produces a low density (below about 600 g/1) detergent composition directly from a surfactant paste and dry starting detergent ingredients. In essence, the process involves agglomerating the starting detergent ingredients in a high speed mixer followed by a second high speed mixer. Thereafter, the agglomerates formed in the high speed mixers are agglomerated and dried in a fluid bed dryer in which a liquid binder is sprayed onto the 20 agglomerates from one or more nozzles at a selected height from the distribution plate of the fluid bed dryer. 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 25 towers which typically emit particulates and volatile organic compounds into the atmosphere.
As used herein, the term "agglomerates" refers to particles formed by agglomerating detergent granules or particles which typically have a smaller median particle size than the formed agglomerates. By "median particle size", it is meant the 30 particle size diameter value above which SO% of the particles have a larger particle size and below which 50% of particles have a smaller particle size. All percentages used herein are expressed as "percent-by-weight" on an anhydrous basis unless indicated otherwise.
In accordance with one aspect of the invention, a process for preparing low density detergent agglomerates is provided. The process comprises the steps of: (a) agglomerating 35 a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates; (b) mixing the agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding the built-up agglomerates into a fluid bed dryer in which a binder is sprayed via a nozzle having a height of from about 2~
cm to about 60 cm from the distributor plate of the fluid bed dryer such that the built-up agglomerates are dried and agglomerated to form the low density detergent agglomerates having a density in a range from about 300 g/1 to about 550 g/1.
In accordance with another aspect of the invention, another process for preparing low density detergent agglomerates is provided. The process comprises the steps of: (a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates; (b) mixing the agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding the built-up agglomerates into a fluid bed dryer in which sodium silicate is sprayed via a nozzle having a height of from about 40 cm to about GO cm from the distributor plate of the fluid bed dryer such that the built-up agglomerates are dried and agglomerated to form the low density detergent agglomerates having a density in a range from about 300 g/1 to about 550 g,~l.
The detergent products made in accordance with any of the process embodiments described herein are also provided.
Accordingly, it is an object of the invention to provide a process for producing a low density detergent composition directly from starting detergent ingredients which does not include relatively expensive specialty ingredients. It is also an object of the invention to provide such a process which is more efficient, flexible and economical so as to facilitate large-scale production of detergents of low as well as high dosage levels.
These and other objects, features and attendant advantages of the present invention will become apparent to those skilled in the art from a reading of the following detailed description of the preferred embodiment and the appended claims.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention is directed to a process in which low density agglomerates are produced by a three step process, the last of which involves a fluid bed dryer containing one or more nozzles positioned at a selected height from the distribution plate of the dryer.
In this way, the process forms free flowing, low density detergent agglomerates which can be used alone as the detergent product or as an admixture with conventional spray-dried detergent granules and/or high density detergent agglomerates in a final commercial detergent product. It should be understood that the process described herein can be operated cpntinuously or in a batch mode depending upon the particularly desired application. One major advantage of the present process is that it utilizes equipment which can be operated differently from the present process parameters to obtain high density detergent compositions. Thus, a single large-scale commercial detergent manufacturing facility can be built to produce high or low density detergent compositions depending upon the local consumer demand and its inevitable fluctuations between compact and non-compact detergent products.
Process In the first step of the process. a detergent surfactant paste or precursor thereof as set forth in more detail hereinafter and dry starting detergent material is inputted and agglomerated in a high speed mixer. Unlike previous processes in this area, the dry starting material can include only those relatively inexpensive detergent materials typically used in modern granular detergent products. Such ingredients, include but are not limited to, builders, fillers, dry surfactants, and flow aides. Preferably, the builder includes aluminosilicates, crystalline layered silicates, phosphates, carbonates and mixtures thereof which is the essential dry starting detergent ingredient within the scope of the current process. Relatively expensive materials such as Burkeite (Na2S04~Na2C03) and the various silicas are not necessary to achieve the desired low density agglomerates produced by the process. Rather, by selecting the binder and nozzle height through which the binder is sprayed onto the agglomerates in the fluid bed dryer as described in more detail hereinafter, the present process achieves the desired low density. Further, it is preferable to include from 1 % to about 40% by weight of undersized detergent particles or "fines" in the first step of the process. This can be conveniently accomplished by screening the detergent particles formed subsequent to the fluid bed dryer to a median particle size range of from about 10 microns to about 150 microns and feeding these "fines" back into the first high speed mixer.
The high speed mixer can be any one of a variety of commercially available mixers TM
such as a Lodige CB 30 mixer or similar brand mixer. These types of mixers essentially consist of a horizontal, hollow static cylinder having a centrally mounted rotating shaft around which several shovel and rod-shaped blades are attached which have a tip speed of from about 5 m/s to about 30 m/s, more preferably from about 6 m/s to about 26 mls.
Preferably, the shaft rotates at a speed of from about 100 rpm to about 2500 rpm, more preferably from about 300 rpm to about 1600 rpm. Preferably, the mean residence time of the detergent ingredients in the high speed mixer is preferably in range from about 2 seconds to about 45 seconds, and most preferably from about 5 seconds to about seconds. This mean residence time is conveniently measured by dividing the weight of the mixer at steady state by throughput (kg/hr) flow. Another suitable mixer is any one of the TM TM
various Flexomix models available from Schugi (Netherlands) which are vertically positioned high speed mixers. This type of mixer is preferably operated at a Froude Index of from about 13 to about 32. See U.S. Patent 5,149,455 to Jacobs et al (issued September 22, 1992) for a detailed discussion of this well-known Froude Index which is a dimensionless number that can be optimally selected by those skilled in the art.
In a prefen;ed embodiment of the process invention, a liquid acid precursor of an anionic surfactant is inputted with the dry starting detergent material which at least includes a neutralizing agent such as sodium carbonate. The preferred liquid acid surfactant precursor is Cl 1-18 linear alkylbenzene sulfonate surfactant ("HLAS"), although any acid precursor of an anionic surfactant may be used in the process. A more preferred embodiment involves feeding a liquid acid precursor of C 12_ 14 linear alkylbenzene sulfonate surfactant with a C10-18 alkyl ethoxylated sulfate ("AS") surfactant into the first high speed mixer, preferably in a weight ratio of from about 5:1 to about 1:~, and most preferably, in a range of from about 1:1 to about 3:1 (HLAS:AS). The result of such mixing is a "dry neutralization" reaction between the HLAS and the sodium carbonate embodied in the dry starting detergent material, all of which forms agglomerates. It is preferable to add the HLAS before the addition of other surfactants such as AS
or alkyl ethoxylate sulfate ("AES") surfactants so as to insure optimal mixing and neutralization of the HLAS in the first high speed mixer. In the second step of the process, the detergent agglomerates formed in the first step are inputted into a second high speed mixer which can be the same piece of equipment as used in the first step or a differern type 1 S of high speed mixer. For example, a Lodige CB mixer can be used in the first step while a Schugi mixer is used in the second step. in this second process step, the agglomerates are mixed and built-up further in a controlled fashion. In this step, a sufficient amount of binder can be inputted to facilitate agglomeration build-up in the mixer.
Typical binders include liquid sodium silicate, a liquid acid precursor of an anionic surfactant such as HLAS, nonionic surfactant, polyethylene glycol or mixtures thereof.
In the next step of the process, the built-up agglomerates are inputted into a fluid bed dryer in which the agglomerates are dried and agglomerated to a median particle size of from about 300 microns to about 700 microns, more preferably from about 325 microns to about 450 microns. The density of the agglomerates formed is from about 300 g/1 to about 550 g/1, more preferably from about 350 g/1 to about 500 gll, and even more preferably from about 400 g/1 to about 480 g/1. All of these densities are generally below that of typical detergent compositions formed of dense agglomerates or most typical spray-dried granules.
A binder as described previously is preferably added during this step to enhance formation of the desired agglomerates. In this regard, a particularly preferred binder is liquid sodium silicate in an amount of from about 0.1% to about 20% by weight of the final low density composition. The nozzle height through which the binder is added is preferably from about 25 cm to about 60 cm, more preferably from about 30 cm to about b0 cm, most preferably from about 40 cm to about 60 cm, and even more preferably at 40 cm, from the distribution plate of the fluid bed dryer. Preferably all of the nozzles used in the fluid bed drying apparatus have such a height arrangement. Unexpectedly, it has been found that by selecting the nozzle height to be within the aforementioned ranges, superior low density agglomerates are produced in the process from both a low density and free flowability standpoint.
Additionally. the benefits of the process in this regard can be enhanced by maintaining the spray-on flux of the binder in the fluid bed to be from about 0.02 kQ. cm2/hr to about 0.06 kg/cm2/hr, more preferably from about 0.04 kg/cm2/hr to about 0.05 ' kg/cm2/hr. Preferably, the air inlet temperature in the fluid bed dryer is from about 100°C
to about 200°C, more preferably from about 110°C to about 130°C. Also, the unfluidized bed height in fluid bed dryer is preferably from about 5 cm to about 20 cm. It has also been found that the process benefits can be enhanced by maintaining the fluidized air flux in the fluid bed dryer is from about 0.6 kg/m2/s to about 0.8 kg/m2/s. It has also been found beneficial to add the binder simultaneously at more than one location in one or more of the steps of the process. For example, the liquid silicate can be added at two locations in the fluid bed dryer, e.g., at or near the inlet port and at or near the exit port.
Also, the median binder droplet diameter is from about 20 microns to about 150 microns, a parameter which enhances formation of the desired built-up agglomerates. Further in this regard, the ratio of the median binder droplet diameter to built-up agglomerate (exiting the second high speed mixer) particle diameter is preferably from about 0.1 to about 0.6.
Optionally, the process may involve adding the binder to both the second high speed mixer as well as the fluid bed dryer. It has also been found beneficial to add the binder simultaneously at more than one location in one or more of the steps of the process.
For example, the liquid silicate can be added at two locations in the fluid bed dryer, e.g., at or near the inlet port and at or near the exit port. As with the first and second steps of the process, the agglomerates are built-up from smaller sizes to large sized particles having a high degree of intraparticie porosity. The degree of intraparticle porosity is preferably from about 20% to about 40%, and most preferably from about 25% to about 35%. The intraparticle porosity can be conveniently measured by standard mercury porosimetry testing.
Other 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 inciude conditioning of the detergent agglomerates by subjecting the agglomerates to additional drying and/or cooling by way of apparatus discussed previously.
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. For example, 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.
Detergent Surfactant Paste or Precursor The liquid acid precursor of anionic surfactant is used in the first step of the process, and in optional embodiments, as a liquid binder in the second and,~or third essential steps of the process. This liquid acid precursor will typically have a viscosity measured at 30°C of from about 500 cps to about 5.000 cps. The liquid acid is a precursor for the anionic surfactants described in more detail hereinafter. A detergent surfactant paste can also be used in the process and is preferably in the form of an aqueous viscous paste, although other 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.' 1. Furthermore, 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. 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. Of the surfactants, anionics and nonionics are preferred and anionics are most preferred.
Nonlimiting examples of the preferred anionic surfactants useful in the surfactant paste, or from which the liquid acid precursor described herein derives, include the conventional C11-Clg alkyl benzene sulfonates ("LAS"), primary, branched-chain and random C10-C20 alkyl sulfates ("AS"), the C10-Clg secondary (2,3) alkyl sulfates of the formula CH3(CH2)x(CHOS03 M+) CH3 and CH3 (CH2)y(CHOS03 M+) CH2CH3 where x and (y + 1 ) are integers of at least about 7, preferably at least about 9, and M is a 510 water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, and the C10-Clg alkyl alkoxy sulfates ("AEXS"; especially EO 1-7 ethoxy sulfates).
Optionally, other exemplary surfactants useful in the paste of the invention include and C 10-C 1 g alkyl alkoxy carboxylates (especially the EO 1-S
ethoxycarboxylates), the C10-18 glycerol ethers, the C10-C1 g alkyl polyglycosides and their corresponding sulfated polyglycosides, and C12-Clg alpha-sulfonated fatty acid esters. If desired, the conventional nonionic and amphoteric surfactants such as the C 12-C 1 g alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and C6-C12 alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxyipropoxy), C 1 ~-C I g betaines and sulfobetaines ("sultaines"), CIO-Clg amine oxides, and the like, can also be included in the overall compositions. The C l p-C 1 g N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C12-C1g N-methylglucamides. See WO
9,206,154.
Other sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C 10-C 1 g N-(3-methoxypropyl) glucamide. The N-propyl through N-hexyl C 12-C 1 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 l0-C 16 soaps may be used.
Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are listed in standard texts.
Dry Detergent Material The starting dry detergent material of the present process preferably comprises a builder and other standard detergent ingredients such as sodium carbonate, especially when a liquid acid precursor of a surfactant is used as it is needed as a neutralizing agent in the I S first step of the process. Thus, preferable starting dry detergent material includes sodium carbonate and a phosphate or an aluminosilicate builder which is referenced as an aluminosilicate ion exchange material. A preferred builder is selected from the group consisting of aluminosilicates, crystalline layered silicates, phosphates, carbonates and mixtures thereof. Preferred phosphate builders include sodium tripolyphosphate, tetrasodium pyrophosphate and mixtwes thereof. Additional specific examples of inorganic phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of from about 6 to 21, and orthophosphates. Examples of polyphosphonate builders are the sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethane 1-hydroxy-1, 1-diphosphonic acid and the sodium and potassium salts of ethane, 1,1,2-triphosphonic 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.
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. In that regard, 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) .
1~
Preferably, the aiuminosilicate 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. Additionally, 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 panicle size diameters which optimize their effectiveness as detergent builders. The term "particle size diameter"
as used herein represents the average particle size diameter of a given aluminosilicate ion exchange material as determined by conventional analytical techniques, such as microscopic l0 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.
Preferably, the aluminosilicate ion exchange material has the formula Naz[(A102)z.( Si02)y]xH20 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 Na 12~~A102) 12~(Si02) 12]~20 wherein x is from about 20 to about 30, preferably about 27. These preferred aluminosilicates are available commercially, for example under designations Zeolite A, Zeolite B and Zeolite X. Alternatively, 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 aluminosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 mg equivalent of CaC03 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaC03 hardness/gram. Additionally, the instant aluminosilicate ion exchange materials are still further character7zed by their calcium ion exchange rate which is at least about 2 grains Ca'+'r/gallon/minute/-gram/gallon, and more preferably in a range from about 2 grains Ca'~/gallon/minute/-gram/gallon to about 6 grains Ca~/gallon/minute/-gram/gallon .
Adiunct Detereent Intredients The starting dry detergent material in the present process can include additional detergent ingredients andlor, any number of additional ingredients can be incorporated in the detergent composition during subsequent steps of the present process.
These adjunct ingredients include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressors, anti-tarnish and anticorrosion 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 _ 3,936.37, issued February 3, 1976 to Baskerville, Jr. et ai .
Other builders can be generally selected from the various borates, polyhydroxy sulfonates, polyacetates, carboxylates, citrates, tarnate mono- and di-succinates, and mixtures thereof. Preferred are the alkali metal, especially sodium, salts of the above. In comparison with amorphous sodium silicates, crystalline layered sodium silicates exhibit a clearly increased calcium and magnesium ion exchange capacity. In addition, 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, however, are generally more expensive than amorphous silicates 1 S 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 ~ NaMSix02x+l.yH20 wherein M is sodium or hydrogen, x is from about 1.9 to about 4 and y is from about 0 to about 20. More preferably, the crystalline layered sodium silicate has the formula NaMSi205.yH20 wherein M is sodium or hydrogen, and y is from about 0 to about 20. These and other crystalline layered sodium silicates are discussed in Corkill et al, U.S.
Patent No.
4,605,509.
Examples of nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of Si02 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.
Examples of 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. Such materials include the water-soluble salts of homo- and copolymers of aliphatic carboxylic l~
acids such as malefic acid, itacontc 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.
Other suitable polycarboxylates 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. 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, convened to the corresponding salt, and added to a detergent composition. Particularly prefer ed polycarboxylate builders are the ether carboxylate builder compositions comprising a combination of tarnate monosuccinate and tarnate disuccinate described in U.S. Patent 4,663,071, Bush et al., issued May 5, 1987.
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. 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. 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.
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~
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.
In order to make the present invention more readily understood, reference is made to the following example, which is intended to be illustrative only and not intended to be limiting in scope.
EXAMPLE
This Example illustrates the process invention in which a low density agglomerated detergent composition is prepared. A Lodige CB 30 high speed mixer is charged with a mixture of powders, namely sodium carbonate (median particle size 15 microns) and sodium tripolyphosphate ("STPP") with a median particle size of 25 microns.
A liquid acid precursor of sodium alkylbenzene sulfonate surfactant (C 12H25-H or "HLAS" as noted below) and a 70% active aqueous C 10_I g alkyl ethoxylated sulfate surfactant (E0 = 3, "AES") paste are also inputted into the Lodige CB 30 mixer, wherein the HLAS is added first. The mixer is operated at 1600 rpm and the sodium carbonate, STPP, HLAS and AES are formed into agglomerates having a median particle size of about 110 microns after a mean residence time in the Lodige CB 30 mixer of about 5 seconds. The agglomerates are then fed to a Schugi (Model # FX160) high speed mixer which is operated at 2800 rpms with a mean residence time of about 2 seconds.
A HLAS
binder is inputted into the Schugi (Model # FX160) mixer during this step which results in built-up agglomerates having a median particle size of about 180 microns being formed.
Thereafter, the built-up agglomerates are passed through a four-zone fluid bed dryer which is operated at an air inlet temperature of about 125°C and a nozzle height of 40 cm from the distribution plate in the first and fourth zones of the fluid bed. The spray-on flux of the sodium silicate in 0.04 kg/cm2/hr, the unfluidized bed height is 10 cm, and the fluidized air flux is 0.6 kg/m2/s. In the amounts and particle size specified below, fines are also added to the Lodige CB 30 mixer. In the first and fourth zones of the fluid bed dryer, liquid sodium silicate is fed into the fluid bed dryer resulting in the finished detergent agglomerates having a density of about 485 g/1 and a median particle size of about 360 microns. Unexpectedly, the finished agglomerates have excellent physical properties in that they are free flowing as exhibited by their superior cake strength grades.
The composition of the agglomerates are given below in Table I.
TABLEI
(% weight) Component I
LAS (Na) 15.8 AES (E0 = 3) 4.7 Sodium carbonate 48.0 STPP 22.7 Sodium Silicate 5.5 Water 3.3 100.0 The agglomerates embody about 14% of fines (less than 150 microns) which are recycled from the fluid bed back into the Lodige CB 30 which enhances production of the agglomerates produced by the process.
~/ J
Having thus described the invention in detail, it will be clear to those skilled in the art that various changes may be made without departing from the scope of the invention and the invention is not to be considered limited to what is described in the specification.
Claims (10)
1. A process for preparing a low density detergent composition characterized by the steps of:
(a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates;
(b) mixing said agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding said built-up agglomerates into a fluid bed dryer in which a binder is sprayed via a nozzle having a height of from 25 cm to 60 cm from the distributor plate of said fluid bed dryer such that said built-up agglomerates are dried and agglomerated to form said low density detergent agglomerates having a density in a range from 300 g/l to 550 g/l.
(a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates;
(b) mixing said agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding said built-up agglomerates into a fluid bed dryer in which a binder is sprayed via a nozzle having a height of from 25 cm to 60 cm from the distributor plate of said fluid bed dryer such that said built-up agglomerates are dried and agglomerated to form said low density detergent agglomerates having a density in a range from 300 g/l to 550 g/l.
2. A process of claim 1 wherein said binder is sodium silicate.
3. A process of claim 1 wherein said binder has a spray-on flux of from 0.02 kg/cm2/hr to 0.06 kg/cm2/hr.
4. A process of claim 1 wherein the air inlet temperature of said fluid bed dryer is from 110°C to 130°C.
5. A process of claim 1 wherein said binder has a median droplet diameter of from 20 microns to 100 microns.
6. A process of claim 1 wherein the fluidized air flux in said fluid bed dryer is from 0.6 kg/m2/s to 0.8 kg/m2/s.
7. A process of claim 1 wherein said step (a) includes agglomerating a liquid acid precursor of C11-18 linear alkylbenzene sulfonate surfactant and a C10-18 alkyl ethoxylated sulfate surfactant.
8. A process of claim 1 wherein said binder is added at the inlet and exit ports of said fluid bed dryer.
9. A process of claim 1 wherein said nozzle height is from 35 cm to 45 cm.
10. A process for preparing a low density detergent composition characterized by the steps of:
(a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates;
(b) mixing said agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding said built-up agglomerates into a fluid bed dryer in which sodium silicate is sprayed via a nozzle having a height of from 40 cm to 60 cm from the distributor plate of said fluid bed dryer such that said built-up agglomerates are dried and agglomerated to form said low density detergent agglomerates having a density in a range from 300 g/l to 550 g/l.
(a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material in a first high speed mixer to obtain agglomerates;
(b) mixing said agglomerates in a second high speed mixer to obtain built-up agglomerates; and (c) feeding said built-up agglomerates into a fluid bed dryer in which sodium silicate is sprayed via a nozzle having a height of from 40 cm to 60 cm from the distributor plate of said fluid bed dryer such that said built-up agglomerates are dried and agglomerated to form said low density detergent agglomerates having a density in a range from 300 g/l to 550 g/l.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US5247297P | 1997-07-14 | 1997-07-14 | |
US60/052,472 | 1997-07-14 | ||
PCT/US1998/014100 WO1999003966A1 (en) | 1997-07-14 | 1998-07-08 | Process for making a low density detergent composition by controlling nozzle height in a fluid bed dryer |
Publications (2)
Publication Number | Publication Date |
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CA2295941A1 CA2295941A1 (en) | 1999-01-28 |
CA2295941C true CA2295941C (en) | 2003-04-22 |
Family
ID=21977821
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA002295941A Expired - Fee Related CA2295941C (en) | 1997-07-14 | 1998-07-08 | Process for making a low density detergent composition by controlling nozzle height in a fluid bed dryer |
Country Status (10)
Country | Link |
---|---|
EP (1) | EP1005522B1 (en) |
JP (1) | JP2003521548A (en) |
CN (1) | CN1170918C (en) |
AR (1) | AR016330A1 (en) |
AT (1) | ATE278765T1 (en) |
BR (1) | BR9810716A (en) |
CA (1) | CA2295941C (en) |
DE (1) | DE69826871T2 (en) |
ES (1) | ES2230707T3 (en) |
WO (1) | WO1999003966A1 (en) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB9526097D0 (en) * | 1995-12-20 | 1996-02-21 | Unilever Plc | Process |
GB9712583D0 (en) | 1997-06-16 | 1997-08-20 | Unilever Plc | Production of detergent granulates |
GB9712580D0 (en) * | 1997-06-16 | 1997-08-20 | Unilever Plc | Production of detergent granulates |
GB9713748D0 (en) * | 1997-06-27 | 1997-09-03 | Unilever Plc | Production of detergent granulates |
ES2184523T3 (en) | 1998-10-26 | 2003-04-01 | Procter & Gamble | PROCEDURES FOR OBTAINING A DETERGENT GRANULAR COMPOSITION THAT HAS AN IMPROVED ASPECT AND SOLUBILITY. |
GB9913546D0 (en) | 1999-06-10 | 1999-08-11 | Unilever Plc | Granular detergent component containing zeolite map and laundry detergent compositions containing it |
DE10258006B4 (en) * | 2002-12-12 | 2006-05-04 | Henkel Kgaa | Dry Neutralization Process II |
EP2123742A1 (en) | 2008-05-14 | 2009-11-25 | The Procter and Gamble Company | A solid laundry detergent composition comprising light density silicate salt |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5335568B2 (en) * | 1973-09-10 | 1978-09-28 | ||
GB2209172A (en) * | 1987-08-28 | 1989-05-04 | Unilever Plc | Preparation of solid particulate components for detergents |
GB9526097D0 (en) * | 1995-12-20 | 1996-02-21 | Unilever Plc | Process |
-
1998
- 1998-07-08 BR BR9810716-0A patent/BR9810716A/en not_active Application Discontinuation
- 1998-07-08 WO PCT/US1998/014100 patent/WO1999003966A1/en active IP Right Grant
- 1998-07-08 CA CA002295941A patent/CA2295941C/en not_active Expired - Fee Related
- 1998-07-08 DE DE69826871T patent/DE69826871T2/en not_active Expired - Fee Related
- 1998-07-08 JP JP2000503174A patent/JP2003521548A/en not_active Withdrawn
- 1998-07-08 EP EP98935559A patent/EP1005522B1/en not_active Expired - Lifetime
- 1998-07-08 ES ES98935559T patent/ES2230707T3/en not_active Expired - Lifetime
- 1998-07-08 AT AT98935559T patent/ATE278765T1/en not_active IP Right Cessation
- 1998-07-08 CN CNB988089513A patent/CN1170918C/en not_active Expired - Fee Related
- 1998-07-13 AR ARP980103395A patent/AR016330A1/en active IP Right Grant
Also Published As
Publication number | Publication date |
---|---|
DE69826871T2 (en) | 2006-03-09 |
WO1999003966A1 (en) | 1999-01-28 |
BR9810716A (en) | 2000-08-08 |
CN1170918C (en) | 2004-10-13 |
CA2295941A1 (en) | 1999-01-28 |
EP1005522B1 (en) | 2004-10-06 |
AR016330A1 (en) | 2001-07-04 |
ATE278765T1 (en) | 2004-10-15 |
EP1005522A1 (en) | 2000-06-07 |
ES2230707T3 (en) | 2005-05-01 |
CN1269824A (en) | 2000-10-11 |
DE69826871D1 (en) | 2004-11-11 |
JP2003521548A (en) | 2003-07-15 |
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