GB2318584A - Process for preparing detergent compositions by spray drying - Google Patents
Process for preparing detergent compositions by spray drying Download PDFInfo
- Publication number
- GB2318584A GB2318584A GB9622272A GB9622272A GB2318584A GB 2318584 A GB2318584 A GB 2318584A GB 9622272 A GB9622272 A GB 9622272A GB 9622272 A GB9622272 A GB 9622272A GB 2318584 A GB2318584 A GB 2318584A
- Authority
- GB
- United Kingdom
- Prior art keywords
- acid
- organic
- alkyl
- preferred
- compositions
- 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.)
- Withdrawn
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 152
- 239000003599 detergent Substances 0.000 title claims abstract description 77
- 238000001694 spray drying Methods 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 7
- 229910010272 inorganic material Inorganic materials 0.000 claims abstract description 21
- 239000011147 inorganic material Substances 0.000 claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 239000011368 organic material Substances 0.000 claims abstract description 16
- -1 alkylbenzene sulphonate Chemical class 0.000 claims description 80
- 239000004094 surface-active agent Substances 0.000 claims description 50
- 238000000034 method Methods 0.000 claims description 34
- 230000008569 process Effects 0.000 claims description 29
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 18
- 229910052783 alkali metal Inorganic materials 0.000 claims description 17
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 15
- 150000001340 alkali metals Chemical class 0.000 claims description 13
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 13
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 9
- 125000000129 anionic group Chemical group 0.000 claims description 9
- 239000003945 anionic surfactant Substances 0.000 claims description 9
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 8
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 8
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 125000002091 cationic group Chemical group 0.000 claims description 5
- 239000003093 cationic surfactant Substances 0.000 claims description 5
- 239000002280 amphoteric surfactant Substances 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- 238000012217 deletion Methods 0.000 claims 1
- 230000037430 deletion Effects 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 description 56
- 239000002243 precursor Substances 0.000 description 33
- 108010065511 Amylases Proteins 0.000 description 32
- 102000013142 Amylases Human genes 0.000 description 32
- 125000000217 alkyl group Chemical group 0.000 description 32
- 150000003839 salts Chemical class 0.000 description 32
- 235000019418 amylase Nutrition 0.000 description 29
- 239000002253 acid Substances 0.000 description 27
- 125000004432 carbon atom Chemical group C* 0.000 description 24
- 239000007844 bleaching agent Substances 0.000 description 23
- 239000000047 product Substances 0.000 description 22
- 102000004190 Enzymes Human genes 0.000 description 21
- 108090000790 Enzymes Proteins 0.000 description 21
- 229940088598 enzyme Drugs 0.000 description 21
- 239000002518 antifoaming agent Substances 0.000 description 20
- 229940025131 amylases Drugs 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 16
- 239000000463 material Substances 0.000 description 16
- 229920001296 polysiloxane Polymers 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 229910001868 water Inorganic materials 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 239000004382 Amylase Substances 0.000 description 13
- 239000002245 particle Substances 0.000 description 13
- 229920000768 polyamine Polymers 0.000 description 13
- 239000003352 sequestering agent Substances 0.000 description 13
- 239000011734 sodium Substances 0.000 description 13
- 238000005406 washing Methods 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 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
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 12
- 150000001204 N-oxides Chemical class 0.000 description 12
- 108091005804 Peptidases Proteins 0.000 description 12
- 102000035195 Peptidases Human genes 0.000 description 12
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 12
- 150000004967 organic peroxy acids Chemical class 0.000 description 12
- 229910052708 sodium Inorganic materials 0.000 description 12
- 238000004061 bleaching Methods 0.000 description 11
- 229920001577 copolymer Polymers 0.000 description 11
- 235000014113 dietary fatty acids Nutrition 0.000 description 11
- 230000000694 effects Effects 0.000 description 11
- 239000000194 fatty acid Substances 0.000 description 11
- 229930195729 fatty acid Natural products 0.000 description 11
- 150000004965 peroxy acids Chemical class 0.000 description 11
- 229920005646 polycarboxylate Polymers 0.000 description 11
- 239000000843 powder Substances 0.000 description 11
- 108090001060 Lipase Proteins 0.000 description 10
- 239000004367 Lipase Substances 0.000 description 10
- 102000004882 Lipase Human genes 0.000 description 10
- 150000007513 acids Chemical class 0.000 description 10
- 150000001768 cations Chemical class 0.000 description 10
- 229910001385 heavy metal Inorganic materials 0.000 description 10
- 235000019421 lipase Nutrition 0.000 description 10
- 239000011572 manganese Substances 0.000 description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 150000004665 fatty acids Chemical class 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 229920000620 organic polymer Polymers 0.000 description 9
- 239000004365 Protease Substances 0.000 description 8
- 150000008051 alkyl sulfates Chemical group 0.000 description 8
- 125000003118 aryl group Chemical group 0.000 description 8
- 229910052748 manganese Inorganic materials 0.000 description 8
- 239000000344 soap Substances 0.000 description 8
- 241000894007 species Species 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 7
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 7
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 230000001590 oxidative effect Effects 0.000 description 7
- 229910052700 potassium Inorganic materials 0.000 description 7
- 239000011591 potassium Substances 0.000 description 7
- 230000002829 reductive effect Effects 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 239000010457 zeolite Substances 0.000 description 7
- YNJSNEKCXVFDKW-UHFFFAOYSA-N 3-(5-amino-1h-indol-3-yl)-2-azaniumylpropanoate Chemical compound C1=C(N)C=C2C(CC(N)C(O)=O)=CNC2=C1 YNJSNEKCXVFDKW-UHFFFAOYSA-N 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000004927 clay Substances 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 239000000975 dye Substances 0.000 description 6
- 125000000623 heterocyclic group Chemical group 0.000 description 6
- 125000001183 hydrocarbyl group Chemical group 0.000 description 6
- 235000019832 sodium triphosphate Nutrition 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 229910021536 Zeolite Inorganic materials 0.000 description 5
- 125000001931 aliphatic group Chemical group 0.000 description 5
- 150000001408 amides Chemical class 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 230000002401 inhibitory effect Effects 0.000 description 5
- 239000003446 ligand Substances 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 5
- 230000000087 stabilizing effect Effects 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 4
- 101710194948 Protein phosphatase PhpP Proteins 0.000 description 4
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 4
- 239000004902 Softening Agent Substances 0.000 description 4
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical class OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 4
- 239000012190 activator Substances 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 125000002723 alicyclic group Chemical group 0.000 description 4
- 125000003342 alkenyl group Chemical group 0.000 description 4
- 125000002877 alkyl aryl group Chemical group 0.000 description 4
- 125000002947 alkylene group Chemical group 0.000 description 4
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 150000007942 carboxylates Chemical class 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 229910001914 chlorine tetroxide Inorganic materials 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 4
- 229910052906 cristobalite Inorganic materials 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 4
- 239000002736 nonionic surfactant Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 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 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 229910052682 stishovite Inorganic materials 0.000 description 4
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 4
- 108010075550 termamyl Proteins 0.000 description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- 239000002888 zwitterionic surfactant Substances 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical class NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 3
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- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 3
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- BGRWYDHXPHLNKA-UHFFFAOYSA-N Tetraacetylethylenediamine Chemical compound CC(=O)N(C(C)=O)CCN(C(C)=O)C(C)=O BGRWYDHXPHLNKA-UHFFFAOYSA-N 0.000 description 3
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- 210000003141 lower extremity Anatomy 0.000 description 3
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- 159000000000 sodium salts Chemical class 0.000 description 3
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- OSSNTDFYBPYIEC-UHFFFAOYSA-N 1-ethenylimidazole Chemical compound C=CN1C=CN=C1 OSSNTDFYBPYIEC-UHFFFAOYSA-N 0.000 description 2
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- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical class O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- XNOQNFJEPBFKLL-UHFFFAOYSA-N butanedioic acid;1,2-diaminopropan-2-ol Chemical compound CC(N)(O)CN.OC(=O)CCC(O)=O.OC(=O)CCC(O)=O XNOQNFJEPBFKLL-UHFFFAOYSA-N 0.000 description 1
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- 239000005018 casein Substances 0.000 description 1
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- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 239000002532 enzyme inhibitor Substances 0.000 description 1
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- XWENCHGJOCJZQO-UHFFFAOYSA-N ethane-1,1,2,2-tetracarboxylic acid Chemical class OC(=O)C(C(O)=O)C(C(O)=O)C(O)=O XWENCHGJOCJZQO-UHFFFAOYSA-N 0.000 description 1
- IGBSXRIJNMDLFB-UHFFFAOYSA-N ethane-1,2-diamine;pentanedioic acid Chemical compound NCCN.OC(=O)CCCC(O)=O.OC(=O)CCCC(O)=O IGBSXRIJNMDLFB-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000007046 ethoxylation reaction Methods 0.000 description 1
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- 159000000011 group IA salts Chemical class 0.000 description 1
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- 229920006158 high molecular weight polymer Polymers 0.000 description 1
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- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical class OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000002563 ionic surfactant Substances 0.000 description 1
- SUMDYPCJJOFFON-UHFFFAOYSA-N isethionic acid Chemical class OCCS(O)(=O)=O SUMDYPCJJOFFON-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 150000003951 lactams Chemical class 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 238000010412 laundry washing Methods 0.000 description 1
- 108010062085 ligninase Proteins 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 239000011683 manganese gluconate Substances 0.000 description 1
- 229940072543 manganese gluconate Drugs 0.000 description 1
- 235000014012 manganese gluconate Nutrition 0.000 description 1
- OXHQNTSSPHKCPB-IYEMJOQQSA-L manganese(2+);(2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Mn+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O OXHQNTSSPHKCPB-IYEMJOQQSA-L 0.000 description 1
- MMIPFLVOWGHZQD-UHFFFAOYSA-N manganese(3+) Chemical compound [Mn+3] MMIPFLVOWGHZQD-UHFFFAOYSA-N 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 108010003855 mesentericopeptidase Proteins 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- KZDZYNUZBPKZKC-UHFFFAOYSA-N n-acetyl-n-[2-(diacetylamino)ethyl]acetamide;hydrogen peroxide Chemical compound OO.CC(=O)N(C(C)=O)CCN(C(C)=O)C(C)=O KZDZYNUZBPKZKC-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- SXLLDUPXUVRMEE-UHFFFAOYSA-N nonanediperoxoic acid Chemical compound OOC(=O)CCCCCCCC(=O)OO SXLLDUPXUVRMEE-UHFFFAOYSA-N 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
- LYRFLYHAGKPMFH-UHFFFAOYSA-N octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(N)=O LYRFLYHAGKPMFH-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 125000000963 oxybis(methylene) group Chemical group [H]C([H])(*)OC([H])([H])* 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- XCRBXWCUXJNEFX-UHFFFAOYSA-N peroxybenzoic acid Chemical class OOC(=O)C1=CC=CC=C1 XCRBXWCUXJNEFX-UHFFFAOYSA-N 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 125000005342 perphosphate group Chemical group 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229940068041 phytic acid Drugs 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 239000000467 phytic acid Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 108010064470 polyaspartate Proteins 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 150000003138 primary alcohols Chemical class 0.000 description 1
- NJKRDXUWFBJCDI-UHFFFAOYSA-N propane-1,1,2,3-tetracarboxylic acid Chemical class OC(=O)CC(C(O)=O)C(C(O)=O)C(O)=O NJKRDXUWFBJCDI-UHFFFAOYSA-N 0.000 description 1
- NJEVMKZODGWUQT-UHFFFAOYSA-N propane-1,1,3,3-tetracarboxylic acid Chemical class OC(=O)C(C(O)=O)CC(C(O)=O)C(O)=O NJEVMKZODGWUQT-UHFFFAOYSA-N 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000001007 puffing effect Effects 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 150000004023 quaternary phosphonium compounds Chemical class 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 238000006268 reductive amination reaction Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 235000012217 sodium aluminium silicate Nutrition 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- ZUFONQSOSYEWCN-UHFFFAOYSA-M sodium;2-(methylamino)acetate Chemical compound [Na+].CNCC([O-])=O ZUFONQSOSYEWCN-UHFFFAOYSA-M 0.000 description 1
- 239000013042 solid detergent Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003890 succinate salts Chemical class 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 229960003080 taurine Drugs 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 150000004026 tertiary sulfonium compounds Chemical class 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- QQOWHRYOXYEMTL-UHFFFAOYSA-N triazin-4-amine Chemical class N=C1C=CN=NN1 QQOWHRYOXYEMTL-UHFFFAOYSA-N 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 210000001364 upper extremity Anatomy 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/02—Preparation in the form of powder by spray drying
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
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 a detergent composition comprises spray drying a slurry of organic and inorganic material, weight ratio of between 0.34 and 0.64 and the slurry having a moisture content of between 25% and 50%. The selection of particular moisture content and ration of organic to inorganic material reduces the tendency to cake.
Description
Detergent Compositions
Technical Field
A process for preparing a detergent composition, said process comprising spray drying a slurry of organic and inorganic material, weight ratio of between 0.34 and 0.64 and said slurry having a moisture content of between 25 % and 50 % .
Background
Cleaning compositions designed for a number of different functions are well known in the art, as reflected by the number of patents in this field.
Traditionally, such cleaning compositions comprise a number of organic and inorganic materials, including for example, a surfactant and a builder.
Inorganic materials commonly employed in, especially granular, detergent compositions include for example an alkali metal or alkaline earth metal sulphate. Sulphate, despite being a common component, does not perform any detersive function and is, in the majority of instances, employed as a filler or bulking agent. It is thus the aim of the present invention to provide a suitable detergent composition comprising a reduced amount of sulphate.
Previously, it has been found that reducing or eliminating the sulphate content of a detergent composition results in the detergent composition being predisposed to 'caking'. Caked products do not flow efficiently and are thus not acceptable to the consumer.
Surprisingly, it has been found that reduced sulphate detergent compositions prepared by the process of the present invention are less predisposed to caking than previously described reduced or nil-sulphate compositions.
The applicants have surprisingly found that caking can be minimised by formulating the detergent composition such that the weight ratio of organic to inorganic material and the moisture content of the slurry of organic and inorganic material in the crutcher (crutcher mix moisture or
CMM) are maintained within a predefined range. In a preferred aspect the detergent compositions prepared by the process of the present invention have density less than 599g/l.
It is further believed that an increase in CMM translates into improved spraying of the slurry into the spray drying tower or atomisability. Whilst it may be expected that this would reduce particle size and therefore increase caking problems, we have surprisingly found that selecting the organic to inorganic ratio and CMM within the predefined limits described herein, potential for caking problems are reduced.
An additional benefit incurred from improved atomisability is the reduction in density of the blown powder collected at the base of the drying tower. The density of the blown powder can also be reduced by injecting air into the organic/inorganic premix slurry. Air injection has an effect akin to steam puffing. An advantage associated with the reduction in density of the detergent compositions prepared by the process of the present invention, is the cost saving incurred by reducing the amount of a component that has little or no detersive action and thus a proportional reduction in transportation cost.
Summarv of the invention
According to the present invention there is provided a process for preparing a detergent composition, said process comprising spray drying a slurry of organic and inorganic material, wherein the ratio of organic to inorganic material is from 0.34 to 0.64, and said slurry having a moisture content of between 25 % and 50%.
Detailed description of the invention
Organic Material
The detergent compositions prepared by the process of the present
invention comprise an organic material. Essentially any organic material is envisaged for use herein. The preferred organic materials used herein are surfactants.
Surfactant
The detergent compositions of the invention contain one or more surfactants selected from anionic, nonionic, non-ester cationic, ampholytic, amphoteric and zwitterionic surfactants and mixtures thereof.
Preferred surfactants for use herein are the anionic surfactants, most preferably Linear alkylbenzene sulfonates (LAS) described below.
The surfactant is preferably present as a component of a surfactant system at a level of from 0. 1% to 50%, more preferably from 1% to 40% by weight, most preferably from 5 % to 30% by weight of the surfactant system.
A typical listing of anionic, nonionic, ampholytic, and zwitterionic classes, and species of these surfactants, is given in U.S.P. 3,929,678 issued to Laughlin and Heuring on December 30, 1975. Further examples are given in "Surface Active Agents and Detergents" (Vol. I and II by
Schwartz, Perry and Berch). A list of suitable cationic surfactants is given in U.S.P. 4,259,217 issued to Murphy on March 31, 1981.
Where present, ampholytic, amphoteric and zwitteronic surfactants are generally used in combination with one or more anionic and/or nonionic surfactants.
Anionic surfactant
Anionic surfactants are preferred components of the compositions prepared by the process of the present invention. Essentially any anionic surfactants useful for detersive purposes are suitable. These can include salts (including, for example, sodium, potassium, ammonium, and substituted ammonium salts such as di- and triethanolamine salts) of the anionic sulfate, sulfonate, carboxylate and sarcosinate surfactants.
Other anionic surfactants include the isethionates such as the acyl isethionates, N-acyl taurates, fatty acid amides of methyl tauride, alkyl succinates and sulfosuccinates, monoesters of sulfosuccinate (especially saturated and unsaturated C12-C18 monoesters) diesters of sulfosuccinate (especially saturated and unsaturated C6-C14 diesters), N-acyl sarcosinates. Resin acids and hydrogenated resin acids are also suitable, such as rosin, hydrogenated rosin, and resin acids and hydrogenated resin acids present in or derived from tallow oil.
Anionic sulfonate surfactant
Preferred anionic surfactants include the anionic sulfonate surfactants suitable for use herein include the salts of C5-C20 linear alkylbenzene sulfonates, alkyl ester sulfonates, C6-C22 primary or secondary alkane sulfonates, C6-C24 olefin sulfonates, sulfonated polycarboxylic acids, alkyl glycerol sulfonates, fatty acyl glycerol sulfonates, fatty oleyl glycerol sulfonates, and any mixtures thereof.
Anionic sulfate surfactant
Anionic sulfate surfactants suitable for use herein include the linear and branched primary and secondary alkyl sulfates, alkyl ethoxysulfates, fatty oleoyl glycerol sulfates, alkyl phenol ethylene oxide ether sulfates, the C-C17 acyl-N-(C1-C4 alkyl) and -N-(C1-C2 hydroxyalkyl) glucamine sulfates, and sulfates of alkylpolysaccharides such as the sulfates of alkylpolyglucoside (the nonionic nonsulfated compounds being described herein).
Alkyl sulfate surfactants are preferably selected from the linear and branched primary C10-Cl8 alkyl sulfates, more preferably the C 11-C 15 branched chain alkyl sulfates and the C12-C14 linear chain alkyl sulfates.
Alkyl ethoxysulfate surfactants are preferably selected from the group consisting of the C 10-C18 alkyl sulfates which have been ethoxylated with from 0.5 to 20 moles of ethylene oxide per molecule. More preferably, the alkyl ethoxysulfate surfactant is a C11-C18, most preferably C 11-C1 5 alkyl sulfate which has been ethoxylated with from 0.5 to 7, preferably from 1 to 5, moles of ethylene oxide per molecule.
A particularly preferred aspect of the invention employs mixtures of the preferred alkyl sulfate and alkyl ethoxymonosulfate surfactants. Such mixtures have been disclosed in PCT Patent Application No. WO 93/18124.
Anionic carboxylate surfactant
Suitable anionic carboxylate surfactants include the alkyl ethoxy carboxylates, the alkyl polyethoxy polycarboxylate surfactants and the soaps ('alkyl carboxyls'), especially certain secondary soaps as described herein.
Suitable alkyl ethoxy carboxylates include those with the formula
RO(CH2CH20)x CH2COO-M+ wherein R is a C6 to C18 alkyl group, x ranges from 0 to 10, and the ethoxylate distribution is such that, on a weight basis, the amount of material where x is 0 is less than 20 % and M is a cation. Suitable alkyl polyethoxy polycarboxylate surfactants include those having the formula RO-(CHR1-CHR2-O)-R3 wherein R is a C6 to
C18 alkyl group, x is from 1 to 25, R1 and R2 are selected from the group consisting of hydrogen, methyl acid radical, succinic acid radical, hydroxysuccinic acid radical, and mixtures thereof, and R3 is selected from the group consisting of hydrogen, substituted or unsubstituted hydrocarbon having between 1 and 8 carbon atoms, and mixtures thereof.
Suitable soap surfactants include the secondary soap surfactants which contain a carboxyl unit connected to a secondary carbon. Preferred secondary soap surfactants for use herein are water-soluble members selected from the group consisting of the water-soluble salts of 2-methyl1-undecanoic acid, 2-ethyl-1-decanoic acid, 2-propyl-1-nonanoic acid, 2butyl-l-octanoic acid and 2-pentyl-1-heptanoic acid. Certain soaps may also be included as suds suppressors.
Alkali metal sarcosinate surfactant
Other suitable anionic surfactants are the alkali metal sarcosinates of formula R-CON (R1) CH2 COOM, wherein R is a C5-C17 linear or branched alkyl or alkenyl group, R1 is a C1-C4 alkyl group and M is an alkali metal ion. Preferred examples are the myristyl and oleoyl methyl sarcosinates in the form of their sodium salts.
Alkoxylated nonionic surfactant
Essentially any alkoxylated nonionic surfactants are suitable herein. The ethoxylated and propoxylated nonionic surfactants are preferred.
Preferred alkoxylated surfactants can be selected from the classes of the nonionic condensates of alkyl phenols, nonionic ethoxylated alcohols, nonionic ethoxylated/propoxylated fatty alcohols, nonionic ethoxylate/propoxylate condensates with propylene glycol, and the nonionic ethoxylate condensation products with propylene oxide/ethylene diamine adducts.
Nonionic alkoxylated alcohol surfactant
The condensation products of aliphatic alcohols with from 1 to 25 moles of alkylene oxide, particularly ethylene oxide and/or propylene oxide, are suitable for use herein. The alkyl chain of the aliphatic alcohol can either be straight or branched, primary or secondary, and generally contains from 6 to 22 carbon atoms. Particularly preferred are the condensation products of alcohols having an alkyl group containing from 8 to 20 carbon atoms with from 2 to 10 moles of ethylene oxide per mole of alcohol.
Nonionic polyhydroxy fatty acid amide surfactant
Polyhydroxy fatty acid amides suitable for use herein are those having the structural formula R2CONR1Z wherein: R1 is H, C 1-C4 hydrocarbyl, 2hydroxy ethyl, 2-hydroxy propyl, ethoxy, propoxy, or a mixture thereof, preferable C1-C4 alkyl, more preferably C1 or C2 alkyl, most preferably
C1 alkyl (i.e., methyl); and R2 is a Cs-C31 hydrocarbyl, preferably straight-chain C-C1g alkyl or alkenyl, more preferably straight-chain
Cg-C17 alkyl or alkenyl, most preferably straight-chain C1 l-Cl7 alkyl or alkenyl, or mixture thereof; and Z is a polyhydroxyhydrocarbyl having a linear hydrocarbyl chain with at least 3 hydroxyls directly connected to the chain, or an alkoxylated derivative (preferably ethoxylated or propoxylated) thereof. Z preferably will be derived from a reducing sugar in a reductive amination reaction; more preferably Z is a glycityl.
Nonionic fatty acid amide surfactant
Suitable fatty acid amide surfactants include those having the formula: R6CON(R7)2 wherein R6 is an alkyl group containing from 7 to 21, preferably from 9 to 17 carbon atoms and each R7 is selected from the group consisting of hydrogen, C 1-C4 alkyl, C1-C4 hydroxyalkyl, and (C2H4O)XH, where x is in the range of from 1 to 3.
Nonionic alkylpolysaccharide surfactant
Suitable alkylpolysaccharides for use herein are disclosed in U.S. Patent 4,565,647, Llenado, issued January 21, 1986, having a hydrophobic group containing from 6 to 30 carbon atoms and a polysaccharide, e.g., a polyglycoside, hydrophilic group containing from 1.3 to 10 saccharide units.
Preferred alkylpolyglycosides have the formula R2O(Cnll2nO)t(glycosyl)x wherein R2 is selected from the group consisting of alkyl, alkylphenyl, hydroxyalkyl, hydroxyalkylphenyl, and mixtures thereof in which the alkyl groups contain from 10 to 18 carbon atoms; n is 2 or 3; t is from 0 to 10, and x is from 1.3 to 8. The glycosyl is preferably derived from glucose.
Amphoteric surfactant
Suitable amphoteric surfactants for use herein include the amine oxide surfactants and the alkyl amphocarboxylic acids.
Suitable amine oxides include those compounds having the formula R3(OR4)xN0(R5)2 wherein R3 is selected from an alkyl, hydroxyalkyl, acylamidopropoyl and alkyl phenyl group, or mixtures thereof, containing from 8 to 26 carbon atoms; R4 is an alkylene or hydroxyalkylene group containing from 2 to 3 carbon atoms, or mixtures thereof; x is from 0 to 5, preferably from 0 to 3; and each R5 is an alkyl or hydroxyalkyl group containing from 1 to 3, or a polyethylene oxide group containing from 1 to 3 ethylene oxide groups. Preferred are C10-Cl8 alkyl dimethylamine oxide, and C 10-18 acylamido alkyl dimethylamine oxide.
A suitable example of an alkyl aphodicarboxylic acid is Miranol(TM)
C2M Conc. manufactured by Miranol, Inc., Dayton, NJ.
Zwitterionic surfactant
Zwitterionic surfactants can also be incorporated into the detergent compositions hereof. These surfactants can be broadly described as derivatives of secondary and tertiary amines, derivatives of heterocyclic secondary and tertiary amines, or derivatives of quaternary ammonium, quaternary phosphonium or tertiary sulfonium compounds. Betaine and sultaine surfactants are exemplary zwitterionic surfactants for use herein.
Suitable betaines are those compounds having the formula
R(R')2N+R2COO- wherein R is a C6-Ci8 hydrocarbyl group, each R1 is typically C1-C3 alkyl, and R2 is a C1-Cs hydrocarbyl group. Preferred betaines are C12-18 dimethyl-ammonio hexanoate and the C10-l8 acylamidopropane (or ethane) dimethyl (or diethyl) betaines. Complex betaine surfactants are also suitable for use herein.
Cationic surfactants
Suitable cationic ester surfactants used in this invention are preferably water dispersible compound having surfactant properties comprising at least one ester (ie -COO-) linkage and at least one cationically charged group.
Other suitable cationic surfactants include the quaternary ammonium surfactants selected from mono C6-C16, preferably C6-C1o N-alkyl or alkenyl ammonium surfactants wherein the remaining N positions are substituted by methyl, hydroxyethyl or hydroxypropyl groups. Other suitable cationic ester surfactants, including choline ester surfactants, have for example been disclosed in US Patents No.s 4228042, 4239660 and 4260529.
Inorganic Material
The compositions prepared by the process of the present invention also include an inorganic material. Essentially any inorganic material is envisaged for use herein. Preferred inorganic marterials used herein are builders, alkali metal and alkali earth metal silicates and sulphates.
The organic to inorganic ratio of the composition prepared by the process of the present invetnion are between 0.34 and 0.6, preferably between 0.343 and 0.555, most preferably between 0.36 and 0.48.
Water-soluble builder compound
The compositions prepared by the process of the present invention preferably contain a detergency builder compound. Suitable builder compound include water-soluble builder compound, typically present at a level of from 1 % to 80% by weight, preferably from 10% to 70% by weight, most preferably from 20% to 60% by weight of the composition.
Suitable water-soluble builder compounds include the water soluble monomeric polycarboxylates, or their acid forms, homo or copolymeric polycarboxylic acids or their salts in which the polycarboxylic acid comprises at least two carboxylic radicals separated from each other by not more that two carbon atoms, borates, phosphates, and mixtures of any of the foregoing.
The carboxylate or polycarboxylate builder can be momomeric or oligomeric in type although monomeric polycarboxylates are generally preferred for reasons of cost and performance.
Suitable carboxylates containing one carboxy group include the water soluble salts of lactic acid, glycolic acid and ether derivatives thereof.
Polycarboxylates containing two carboxy groups include the water-soluble salts of succinic acid, malonic acid, (ethylenedioxy) diacetic acid, maleic acid, diglycolic acid, tartaric acid, tartronic acid and fumaric acid, as well as the ether carboxylates and the sulfinyl carboxylates. Polycarboxylates containing three carboxy groups include, in particular, water-soluble citrates, aconitrates and citraconates as well as succinate derivatives such as the carboxymethyloxysuccinates described in British Patent No.
1,379,241, lactoxysuccinates described in British Patent No. 1,389,732, and aminosuccinates described in Netherlands Application 7205873, and the oxypolycarboxylate materials such as 2-oxa-1,1,3-propane tricarboxylates described in British Patent No. 1,387,447.
Polycarboxylates containing four carboxy groups include oxydisuccinates disclosed in British Patent No. 1,261,829, 1,1 ,2,2-ethane tetracarboxylates, 1,1,3,3-propane tetracarboxylates and 1,1,2,3-propane tetracarboxylates. Polycarboxylates containing sulfo substituents include the sulfosuccinate derivatives disclosed in British Patent Nos. 1,398,421 and 1,398,422 and in U.S. Patent No. 3,936,448, and the sulfonated pyrolysed citrates described in British Patent No. 1,439,000. Preferred polycarboxylates are hydroxycarboxylates containing up to three carboxy groups per molecule, more particularly citrates.
The parent acids of the monomeric or oligomeric polycarboxylate chelating agents or mixtures thereof with their salts, e.g. citric acid or citrate/citric acid mixtures are also contemplated as useful builder components.
Borate builders, as well as builders containing borate-forming materials that can produce borate under detergent storage or wash conditions are useful water-soluble builders herein.
Suitable examples of water-soluble phosphate builders are the alkali metal tripolyphosphates, sodium, potassium and ammonium pyrophosphate, sodium and potassium and ammonium pyrophosphate, sodium and potassium orthophosphate, sodium polymeta/phosphate in which the degree of polymerization ranges from about 6 to 21, and salts of phytic acid.
Partially soluble or insoluble builder compound
Other suitable builder compounds include the partially soluble or insoluble builder compounds, typically present at a level of from 1 % to 80% by weight, preferably from 10% to 70% by weight, most preferably from 20 % to 60% weight of the composition.
Examples of largely water insoluble builders include the sodium aluminosilicates.
Suitable aluminosilicate zeolites have the unit cell formula Naz[(AlO2)z(SiO2)y]. xH2O wherein z and y are at least 6; the molar ratio of z toy is from 1.0 to 0.5 and xis at least 5, preferably from 7.5 to 276, more preferably from 10 to 264. The aluminosilicate material are in hydrated form and are preferably crystalline, containing from 10% to 28 % , more preferably from 18% to 22% water in bound form.
The aluminosilicate zeolites can be naturally occurring materials, but are preferably synthetically derived. Synthetic crystalline aluminosilicate ion exchange materials are available under the designations Zeolite A, Zeolite
B, Zeolite P, Zeolite X, Zeolite HS and mixtures thereof. Zeolite A has the formula
Na 12 [Alo2) 12 (SiO2)12]. xH2O wherein x is from 20 to 30, especially 27. Zeolite X has the formula
Na86 [(A102)86(Si02)106] 276 H2O. Zeolite MAP, as disclosed in EP
B-384,070 is a preferred zeolite builder herein.
Alkalinity svstem
Additional suitable inorganic materials also inlcude those used as components of the alkalinity system. The alkalinity system were present is at levels of from 1.5 % to 95 %, preferably from 5 % to 60%, most preferably from 10% to 40% by weight of the composition Components of an alkalinity system comprise components capable of providing alkalinity species in solution. By alkalinity species it is meant for the purposes of this invention: carbonate, bicarbonate, hydroxide and the various silicate anions. Such alkalinity species can be formed for example, when alkaline salts selected from alkali metal or alkaline earth carbonate, bicarbonate, hydroxide or silicate, including crystalline layered silicate, salts and any mixtures thereof are dissolved in water. Alkali metal silicate salts are preferred components of the detergent cmpositions prepared herein.
Sulphate
The compositions prepared by the process of the present invention preferably contain an alkali metal or alkali earth metal sulphate. A preferred sulphate used herein is anhydrous sodium sulphate.
Preparation of the Detergent composition
The compositions of the present invention are prepared in a two stage conventional spray drying process. Stage one comprises mixing the organic and inorganic materials in a conventional large blender-type piece of equipment, commonly known as a crutcher. The resulting premix is in the form of a slurry having a moisture content (crutcher mix moisture or
CMM) of between 25 % and 50%, preferably between 30 and 45 % , most preferably between 34 % and 43 %. The slurry is pumped to a height, such that it can be sprayed into the spray drying tower of stage two.
The spray drying tower is heated to between 80 and 350"C. As the organic and inorganic materials in the slurry fall in the tower, moisture is driven off. Eventually particles of organic and inorganic material collect at the base of the tower. Particles formed in the spray drying tower are known as blown powder. In an additional stage, any remaining components of the detergent composition may be dry mixed with or sprayed onto the blown powder.
All equipment used in the crutching and spray drying process are conventional. Variations of this process are also envisaged. In a preferres embodiment of the present invention air is injected into the crutcher mix before it is sprayed into the spray drying tower.
Additional detergent components
The additional organic or inorganic detergent components listed below may be incorporated into the detergent composition. Where the additional components are included as part of the slurry intended for forming the blown powder, they are also to be included for calculation of the organic to inorganic ratio.
The detergent compositions prepared by the process of the present invention may contain a variety of additional detergent components. The precise nature of these components, and levels of incorporation thereof will depend on the physical form of the composition, and the precise nature of the washing operation for which it is to be used.
The compositions of the invention preferably contain one or more detergent components selected from additional surfactants, additional builders, alkalinity system, bleach, organic polymeric compounds, enzymes, enzyme stabilising system, suds suppressors, lime soap dispersants, soil suspension and anti-redeposition agents and corrosion inhibitors.
Organic peroxyacid bleaching system
A optional feature of detergent compositions prepared herein, is an organic peroxyacid bleaching system. In one preferred execution the bleaching system contains a hydrogen peroxide source and an organic peroxyacid bleach precursor compound. The production of the organic peroxyacid occurs by an in situ reaction of the precursor with a source of hydrogen peroxide. Preferred sources of hydrogen peroxide include inorganic perhydrate bleaches. In an alternative preferred execution a preformed organic peroxyacid is incorporated directly into the composition. Compositions containing mixtures of a hydrogen peroxide source and organic peroxyacid precursor in combination with a preformed organic peroxyacid are also envisaged.
Inorganic perhydrate bleaches
Inorganic perhydrate salts are a preferred source of hydrogen peroxide.
These salts are normally incorporated in the form of the alkali metal, preferably sodium salt at a level of from 1 % to 40% by weight, more preferably from 2% to 30% by weight and most preferably from 5 % to 25 % by weight of the compositions.
Examples of inorganic perhydrate salts include perborate, percarbonate, perphosphate, persulfate and persilicate salts. The inorganic perhydrate salts are normally the alkali metal salts. The inorganic perhydrate salt may be included as the crystalline solid without additional protection. For certain perhydrate salts however, the preferred executions of such granular compositions utilize a coated form of the material which provides better storage stability for the perhydrate salt in the granular product. Suitable coatings comprise inorganic salts such as alkali metal silicate, carbonate or borate salts or mixtures thereof, or organic materials such as waxes, oils, or fatty soaps.
Sodium perborate is a preferred perhydrate salt and can be in the form of the monohydrate of nominal formula NaB02H202 or the tetrahydrate NaB02H202 .3 3 H20.
Alkali metal percarbonates, particularly sodium percarbonate are preferred perhydrates herein. Sodium percarbonate is an addition compound having a formula corresponding to 2Na2CO3.3H202, and is available commercially as a crystalline solid.
Potassium peroxymonopersulfate is another inorganic perhydrate salt of use in the detergent compositions herein.
Peroxyacid bleach precursor
Peroxyacid bleach precursors are compounds which react with hydrogen peroxide in a perhydrolysis reaction to produce a peroxyacid. Generally peroxyacid bleach precursors may be represented as
where L is a leaving group and X is essentially any functionality, such that on perhydroloysis the structure of the peroxyacid produced is
Peroxyacid bleach precursor compounds are preferably incorporated at a level of from 0.5% to 20% by weight, more preferably from 1 % to 15% by weight, most preferably from 1.5% to 10% by weight of the detergent compositions.
Suitable peroxyacid bleach precursor compounds typically contain one or more N- or O-acyl groups, which precursors can be selected from a wide range of classes. Suitable classes include anhydrides, esters, imides, lactams and acylated derivatives of imidazoles and oximes. Examples of useful materials within these classes are disclosed in GB-A-1586789.
Suitable esters are disclosed in GB-A-836988, 864798, 1147871, 2143231 and EP-A-0170386.
Leaving groups
The leaving group, hereinafter L group, must be sufficiently reactive for the perhydrolysis reaction to occur within the optimum time frame (e.g., a wash cycle). However, if L is too reactive, this activator will be difficult to stabilize for use in a bleaching composition.
Preferred L groups are selected from the group consisting of:
and mixtures thereof, wherein R1 is an alkyl, aryl, or alkaryl group containing from 1 to 14 carbon atoms, R3is an alkyl chain containing from 1 to 8 carbon atoms, R4 is H or R3, and Y is H or a solubilizing group. Any of R1, R3 and R4 may be substituted by essentially any functional group including, for example alkyl, hydroxy, alkoxy, halogen, amine, nitrosyl, amide and ammonium or alkyl ammmonium groups
The preferred solubilizing groups are -SO3-M +, -CO2-M +, -SO4 +, -N + )LX- and O < --N(R3)3 and most preferably -SO3-M+ and -CO2-M wherein R3 is an alkyl chain containing from 1 to 4 carbon atoms, M is a cation which provides solubility to the bleach activator and
X is an anion which provides solubility to the bleach activator.
Preferably, M is an alkali metal, ammonium or substit wherein R1 is an alkyl group with from 1 to 14 carbon atoms, R2 is an alkylene group containing from 1 to 14 carbon atoms, and R5 is H or an alkyl group containing 1 to 10 carbon atoms and L can be essentially any leaving group. Amide substituted bleach activator compounds of this type are described in EP-A-0170386.
Perbenzoic acid precursor
Perbenzoic acid precursor compounds provide perbenzoic acid on perhydrolys is. Suitable O-acylated perbenzoic acid precursor compounds include the substituted and unsubstituted benzoyl oxybenzene sulfonates, and the benzoylation products of sorbitol, glucose, and all saccharides with benzoylating agents, and those of the imide type including N-benzoyl succinimide, tetrabenzoyl ethylene diamine and the N-benzoyl substituted ureas. Suitable imidazole type perbenzoic acid precursors include Nbenzoyl imidazole and N-benzoyl benzimidazole. Other useful N-acyl group-containing perbenzoic acid precursors include N-benzoyl pyrrolidone, dibenzoyl taurine and benzoyl pyroglutamic acid.
Cationic peroxyacid precursors
Cationic peroxyacid precursor compounds produce cationic peroxyacids on perhydrolysis.
Typically, cationic peroxyacid precursors are formed by substituting the peroxyacid part of a suitable peroxyacid precursor compound with a positively charged functional group, such as an ammonium or alkyl ammonium group, preferably an ethyl or methyl ammonium group.
Cationic peroxyacid precursors are typically present in the solid detergent compositions as a salt with a suitable anion, such as a halide ion.
The peroxyacid precursor compound to be so cationically substituted may be a perbenzoic acid, or substituted derivative thereof, precursor compound as described hereinbefore. Alternatively, the peroxyacid precursor compound may be an alkyl percarboxylic acid precursor compound or an amide substituted alkyl peroxyacid precursor as described hereinafter
Cationic peroxyacid precursors are described in U.S. Patents 4,904,406; 4,751,015; 4,988,451; 4,397,757; 5,269,962; 5,127,852; 5,093,022; 5,106,528; U.K. 1,382,594; EP 475,512, 458,396 and 284,292; and in
JP 87-318,332.
Examples of preferred cationic peroxyacid precursors are described in
UK Patent Application No. 9407944.9 and US Patent Application Nos.
08/298903, 08/298650, 08/298904 and 08/298906.
Suitable cationic peroxyacid precursors include any of the ammonium or alkyl ammonium substituted alkyl or benzoyl oxybenzene sulfonates, Nacylated caprolactams, and monobenzoyltetraacetyl glucose benzoyl peroxides. Preferred cationic peroxyacid precursors of the N-acylated caprolactam class include the trialkyl ammonium methylene benzoyl caprolactams and the trialkyl ammonium methylene alkyl caprolactams.
Benzoxazin organic peroxyacid precursors
Also suitable are precursor compounds of the benzoxazin-type, as disclosed for example in EP-A-332,294 and EP-A-482,807, particularly those having the formula:
wherein R1 is H, alkyl, alkaryl, aryl, or arylalkyl.
Preformed organic peroxyacid
The organic peroxyacid bleaching system may contain, in addition to, or as an alternative to, an organic peroxyacid bleach precursor compound, a preformed organic peroxyacid, typically at a level of from 1 % to 15 % by weight, more preferably from 1 % to 10% by weight of the composition.
A preferred class of organic peroxyacid compounds are the amide substituted compounds of the following general formulae:
wherein R1 is an alkyl, aryl or alkaryl group with from 1 to 14 carbon atoms, R2 is an alkylene, arylene, and alkarylene group containing from 1 to 14 carbon atoms, and R5 is H or an alkyl, aryl, or alkaryl group containing 1 to 10 carbon atoms. Amide substituted organic peroxyacid compounds of this type are described in EP-A-0170386.
Other organic peroxyacids include diacyl and tetraacylperoxides, especially diperoxydodecanedioc acid, diperoxytetradecanedioc acid and diperoxyhexadecanedioc acid. and diperazelaic acid, and diperbrassylic acid and N-phthaloylaminoperoxicaproic acid are also suitable herein.
Bleach catalyst
The compositions optionally contain a transition metal containing bleach catalyst. One suitable type of bleach catalyst is a catalyst system comprising a heavy metal cation of defined bleach catalytic activity, such as copper, iron, cobalt or manganese cations, an auxiliary metal cation having little or no bleach catalytic activity, such as zinc or aluminum cations, and a sequestrant having defined stability constants for the catalytic and auxiliary metal cations, particularly ethylenediaminetetraacetic acid, ethylenediaminetetre (methylenephosphonic acid) and water-soluble salts thereof. Such catalysts are disclosed in U.S. Pat. 4,430,243.
Other types of bleach catalysts include the manganese-based complexes disclosed in U.S. Pat. 5,246,621 and U.S. Pat. 5,244,594. Preferred examples of these catalysts include MnIV2(u-0)3(1 ,4,7-trimethyl-l ,4,7- triazacyclononane)2-(PF6)2, MnIII2(u-O)1(u-OAc)2(1,7,7-trimethyl1,4,7-triazacyclononane)2-(ClO4)2, MnIV4(u-O)6(1,4,7- triazacyclononane)4-(ClO4)2, MnIIIMnIV4(u-O)1(u-OAc)2-(1,4,7- trimethyl-1,4,7-triazacyclononane)2-(Cl04)3, and mixtures thereof.
Others are described in European patent application publication no.
549,272. Other ligands suitable for use herein include 1 ,5,9-trimethyl- 1,5,9-triazacyclododecane, 2-methyl-1,4,7-triazacyclononane, 2-methyl 1,4, 7-triazacyclononane, 1,2,4,7-tetramethyl-1,4,7-triazacyclononane, and mixtures thereof.
For examples of suitable bleach catalysts see U.S. Pat. 4,246,612 and
U.S. Pat. 5,227,084. See also U.S. Pat. 5,194,416 which teaches mononuclear manganese (IV) complexes such as Mn(1,4,7-trimethyl- 1 ,4,7-triazacyclononane)(OCH3)3,(PF6) . Still Still another type of bleach catalyst, as disclosed in U.S. Pat. 5,114,606, is a water-soluble complex of manganese (III), and/or (IV) with a ligand which is a non-carboxylate polyhydroxy compound having at least three consecutive C-OH groups.
Other examples include binuclear Mn complexed with tetra-N-dentate and bi-N-dentate ligands, including N4MnIII(uO)2MnIVN4) + and [Bipy2MnIII(u-O)2MnIVbipy2]-(ClO4)3.
Further suitable bleach catalysts are described, for example, in European patent application No. 408,131 (cobalt complex catalysts), European patent applications, publication nos. 384,503, and 306,089 (metalloporphyrin catalysts), U.S. 4,728,455 (manganese/multidentate ligand catalyst), U.S. 4,711,748 and European patent application, publication no. 224,952, (absorbed manganese on aluminosilicate catalyst), U.S.
4,601,845 (aluminosilicate support with manganese and zinc or magnesium salt), U.S. 4,626,373 (manganese/ligand catalyst), U.S.
4,119,557 (ferric complex catalyst), German Pat. specification 2,054,019 (cobalt chelant catalyst) Canadian 866,191 (transition metal-containing salts), U.S. 4,430,243 (chelants with manganese cations and non-catalytic metal cations), and U.S. 4,728,455 (manganese gluconate catalysts).
Enzvme
Suitable enzymatic materials include the commercially available lipases, cutinases, amylases, neutral and alkaline proteases, esterases, cellulases, pectinases, lactases and peroxidases conventionally incorporated into detergent compositions. Preferred enzymes are discussed in US Patents 3,519,570 and 3,533,139.
Enzymes are normally incorporated into detergent or detergent additive compositions at levels sufficient to provide a "cleaning-effective amount".
The term "cleaning effective amount" refers to any amount capable of producing a cleaning, stain removal, whitening, deodorizing, or freshness improving effect on substrates. In practical terms for current commercial preparations, typical amounts are up to 5 mg by weight, more typically 0.01 mg to 3 mg, of active enzyme per gram of the detergent composition. Stated otherwise, the compositions herein will typically comprise from 0.001 % to 5%, preferably from 0.01 % to 1 % by weight of a commercial enzyme preparation.
Preferred commercially available protease enzymes include those sold under the tradenames Alcalase, Savinase, Primase, Durazym, and
Esperase by Novo Industries A/S (Denmark), those sold under the tradename Maxatase, Maxacal and Maxapem by Gist-Brocades, those sold by Genencor International, and those sold under the tradename
Opticlean and Optimase by Solvay Enzymes. As well as Protease A as disclosed in EP 130,756 A, January 9, 1985 and Protease B as disclosed in EP 303,761 A, April 28, 1987 and EP 130,756 A, January 9, 1985.
See also a high pH protease from Bacillus sp. NCIMB 40338 described in
WO 9318140 A to Novo. Enzymatic detergents comprising protease, one or more other enzymes, and a reversible protease inhibitor are described in WO 9203529 A to Novo. Other preferred proteases include those of WO 9510591 A to Procter & Gamble. When desired, a protease having decreased absorption and increased hydrolysis is available as described in WO 9507791 to Procter and Gamble. A recombinant trypsin-like protease for detergents suitable herein is described in WO 9425583 to Novo.
In more detail, an especially preferred protease, referred to as "Protease
D" is a carbonyl hydrolase variant having an amino acid sequence not found in nature,which is derived from a precursor carbonyl hydrolase by substituting a different amino acid for a plurality of amino acid residues at a position in said carbonyl hydrolase equivalent to position +76, preferably also in combination with one or more amino acid residue positions equivalent to those selected from the group consisting of + 99, +101, +103, +104, +107, +123, +27, +105, +109, +126, +128, +135, +156, +166, +195, +197, +204, +206, +210, +210, +216, +217, +218, +222, +260, +265, and/or +274 according to the numbering of Bacillus amyloliquefaciens subtilisin, as described in the patent applications of A. Baeck, et al, entitled "Protease-Containing
Cleaning Compositions" having US Serial No. 08/322,676, and C Ghosh, et al, "Bleaching Compositions Comprising Protease Enzymes" having
US Serial No. 08/322,677, both filed October 13, 1994.
Protease enzyme may be incorporated into the compositions in accordance with the invention at a level of from 0.0001 % to 4 % active enzyme by weight of the composition.
Preferred amylases include, for example, amylases obtained from a special strain of B licheniformis, described in more detail in GB1,269,839 (Novo). Preferred commercially available amylases include for example, those sold under the tradename Rapidase by Gist-Brocades, and those sold under the tradename Termamyl fungamyl and BAN by
Novo Industries A/S.
Engineering of enzymes for improved stability, e.g., oxidative stability, is known. See, for example J. Biological Chem., Vol. 260, No. 11, June 1985, pp. 6518-6521. Certain preferred embodiments of the present compositions can make use of amylases having improved stability in detergents such as automatic dishwashing types, especially improved oxidative stability as measured against a reference-point of TERMAMYL (E) in commercial use in 1993. These preferred amylases herein share the characteristic of being "stability-enhanced" amylases, characterized, at a minimum, by a measurable improvement in one or more of: oxidative stability, e.g., to hydrogen peroxide / tetraacetylethylenediamine in buffered solution at pH 9-10; thermal stability, e.g., at common wash temperatures such as about 60"C; or alkaline stability, e.g., at a pH from about 8 to about 11, measured versus the above-identified reference-point amylase. Stability can be measured using any of the art-disclosed technical tests. See, for example, references disclosed in WO 9402597.
Stability-enhanced amylases can be obtained from Novo or from
Genencor International. One class of highly preferred amylases herein have the commonality of being derived using site-directed mutagenesis from one or more of the Bacillus amylases, especially the Bacillus aamylases, regardless of whether one, two or multiple amylase strains are the immediate precursors. Oxidative stability-enhanced amylases vs. the above-identified reference amylase are preferred for use, especially in bleaching, more preferably oxygen bleaching, as distinct from chlorine bleaching, detergent compositions herein. Such preferred amylases include (a) an amylase according to the hereinbefore incorporated WO 9402597, Novo, Feb. 3, 1994, as further illustrated by a mutant in which substitution is made, using alanine or threonine, preferably threonine, of the methionine residue located in position 197 of the B. licheniformis alpha-amylase, known as TERMAMYL8 or the homologous position variation of a similar parent amylase, such as B. amyloliquefaciens, B.
subtilis, or B. stearothennophilus; (b) stability-enhanced amylases as described by Genencor International in a paper entitled "Oxidatively
Resistant alpha-Amylases" presented at the 207th American Chemical
Society National Meeting, March 13-17 1994, by C. Mitchinson. Therein it was noted that bleaches in automatic dishwashing detergents inactivate alpha-amylases but that improved oxidative stability amylases have been made by Genencor from B licheniformis NCIB8061. Methionine (Met) was identified as the most likely residue to be modified. Met was substituted, one at a time, in positions 8, 15, 197, 256, 304, 366 and 438 leading to specific mutants, particularly important being M197L and
M197T with the M197T variant being the most stable expressed variant.
Stability was measured in CASCADE8 and SUNLIGHTB; (c) particularly preferred amylases herein include amylase variants having additional modification in the immediate parent as described in WO 9510603 A and are available from the assignee, Novo, as DURAMYL.
Other particularly preferred oxidative stability enhanced amylase include those described in WO 9418314 to Genencor International and WO 9402597 to Novo. Any other oxidative stability-enhanced amylase can be used, for example as derived by site-directed mutagenesis from known chimeric, hybrid or simple mutant parent forms of available amylases.
Other preferred enzyme modifications are accessible. See WO 9509909
A to Novo.
Other amylase enzymes include those described in WO 95/26397 and in co-pending application by Novo Nordisk PCT/DK96/00056. Specific amylase enzymes for use in the detergent compositions of the present invention include amylases characterized by having a specific activity at least 25 % higher than the specific activity of Termamyl(D at a temperature range of 25"C to 550C and at a pH value in the range of 8 to 10, measured by the PhadebasX a-amylase activity assay. (Such PhadebasX a-amylase activity assay is described at pages 9-10, WO 95/26397.) Also included herein are amylases which are at least 80% homologous with the amino acid sequences shown in the SEQ ID listings in the references.
Amylase enzyme may be incorporated into the composition in accordance with the invention at a level of from 0.0001 % to 2% active enzyme by weight of the composition.
Lipolytic enzyme may be present at levels of active lipolytic enzyme of from 0.0001% to 2% by weight, preferably 0.001% to 1% by weight, most preferably from 0.001 % to 0.5% by weight of the compositions.
The lipase may be fungal or bacterial in origin being obtained, for example, from a lipase producing strain of Humicola sp., Thermomyces sp. or Pseudomonas sp. including Pseudomonas pseudoalcaligenes or
Pseudomas fluorescens. Lipase from chemically or genetically modified mutants of these strains are also useful herein. A preferred lipase is derived from Pseudomonas pseudoalcaligenes, which is described in
Granted European Patent, EP-B-0218272.
Another preferred lipase herein is obtained by cloning the gene from
Humicola lanuginosa and expressing the gene in Aspergillus oryza, as host, as described in European Patent Application, EP-A-0258 068, which is commercially available from Novo Industri A/S, Bagsvaerd, Denmark, under the trade name Lipolase. This lipase is also described in U.S.
Patent 4,810,414, Huge-Jensen et al, issued March 7, 1989.
Cutinase enzymes suitable for use herein are described in WO 8809367 A to Genencor.
Peroxidase enzymes may be used in combination with oxygen sources, e.g., percarbonate, perborate, hydrogen peroxide, etc., for "solution bleaching" or prevention of transfer of dyes or pigments removed from substrates during the wash to other substrates present in the wash solution. Known peroxidases include horseradish peroxidase, ligninase, and haloperoxidases such as chloro- or bromo-peroxidase. Peroxidasecontaining detergent compositions are disclosed in WO 89099813 A,
October 19, 1989 to Novo and WO 8909813 A to Novo.
Enzvme Stabilizing System
A preferred component of enzyme-containing compositions is an enzyme stabilising system. When present the enzyme stabilising system is at levels of from 0.001 % to 10%, preferably from 0.005 % to 8 %, most preferably from 0.01 % to 6%, by weight of the composition. The enzyme stabilizing system can be any stabilizing system which is compatible with the detersive enzyme. Such stabilizing systems can comprise calcium ion, boric acid, propylene glycol, short chain carboxylic acid, boronic acid, chlorine bleach scavengers and mixtures thereof. Such stabilizing systems can also comprise reversible enzyme inhibitors, such as reversible protease inhibitors.
Heavy metal ion sequestrant
The detergent compositions prepared by the process of the invention preferably contain as an optional component a heavy metal ion sequestrant. By heavy metal ion sequestrant it is meant herein components which act to sequester (chelate) heavy metal ions. These components may also have calcium and magnesium chelation capacity, but preferentially they show selectivity to binding heavy metal ions such as iron, manganese and copper.
Heavy metal ion sequestrants are generally present at a level of from 0.005 % to 20%, preferably from 0.1% to 10%, more preferably from 0.25% to 7.5 % and most preferably from 0.5% to 5 % by weight of the compositions.
Suitable heavy metal ion sequestrants for use herein include organic phosphonates, such as the amino alkylene poly (alkylene phosphonates), alkali metal ethane 1 hydroxy disphosphonates and nitrilo trimethylene phosphonates.
Preferred among the above species are diethylene triamine penta (methylene phosphonate), ethylene diamine tri (methylene phosphonate) hexamethylene diamine tetra (methylene phosphonate) and hydroxyethylene 1,1 diphosphonate.
Other suitable heavy metal ion sequestrant for use herein include nitrilotriacetic acid and polyaminocarboxylic acids such as ethylenediaminotetracetic acid, ethylenetriamine pentacetic acid, ethylenediamine disuccinic acid, ethylenediamine diglutaric acid, 2hydroxypropylenediamine disuccinic acid or any salts thereof. Especially preferred is ethylenediamine-N,N'-disuccinic acid (EDDS) or the alkali metal, alkaline earth metal, ammonium, or substituted ammonium salts thereof, or mixtures thereof.
Other suitable heavy metal ion sequestrants for use herein are iminodiacetic acid derivatives such as 2-hydroxyethyl diacetic acid or glyceryl imino diacetic acid, described in EP-A-317,542 and EP-A399,133. The iminodiacetic acid-N-2-hydroxypropyl sulfonic acid and aspartic acid N-carboxymethyl N-2-hydroxypropyl-3 -sulfonic acid sequestrants described in EP-A-516,102 are also suitable herein. The - alanine-N,N'-diacetic acid, aspartic acid-N,N'diacetic acid, aspartic acid
N-monoacetic acid and iminodisuccinic acid sequestrants described in EP
A-509,382 are also suitable.
EP-A476,257 describes suitable amino based sequestrants. EP-A510,331 describes suitable sequestrants derived from collagen, keratin or casein. EP-A-528,859 describes a suitable alkyl iminodiacetic acid sequestrant. Dipicolinic acid and 2-phosphonobutane-1,2,4-tricarboxylic acid are also suitable. Glycinamide-N,N'-disuccinic acid (GADS), ethylenediamine -N-N' -diglutaric acid (EDDG) and 2 hydroxypropylenediamine-N-N'-disuccinic acid (HPDDS) are also suitable.
Organic polymeric compound
Organic polymeric compounds are optional components of the detergent compositions prepared in accord with the invention, and are preferably present as components of any particulate components where they may act such as to bind the particulate component together. By organic polymeric compound it is meant herein essentially any polymeric organic compound commonly used as dispersants, and anti-redeposition and soil suspension agents in detergent compositions, including any of the high molecular weight organic polymeric compounds described as clay flocculating agents herein.
Organic polymeric compound is typically incorporated in the detergent compositions of the invention at a level of from 0.1 % to 30%, preferably from 0.5% to 15%, most preferably from 1% to 10% by weight of the compositions.
Examples of organic polymeric compounds include the water soluble organic homo- or co-polymeric polycarboxylic acids or their salts in which the polycarboxylic acid comprises at least two carboxyl radicals separated from each other by not more than two carbon atoms. Polymers of the latter type are disclosed in GB-A-1,596,756. Examples of such salts are polyacrylates of MWt 2000-5000 and their copolymers with maleic anhydride, such copolymers having a molecular weight of from 20,000 to 100,000, especially 40,000 to 80,000.
The polyamino compounds are useful herein including those derived from aspartic acid such as those disclosed in EP-A-305282, EP-A-305283 and EP-A-35 1629.
Terpolymers containing monomer units selected from maleic acid, acrylic acid, polyaspartic acid and vinyl alcohol, particularly those having an average molecular weight of from 5,000 to 10,000, are also suitable herein.
Other organic polymeric compounds suitable for incorporation in the detergent compositions herein include cellulose derivatives such as methylcellulose, carboxymethylcellulose, hydroxypropylmethylcellulose and hydroxyethylcellulose.
Further useful organic polymeric compounds are the polyethylene glycols, particularly those of molecular weight 1000-10000, more particularly 2000 to 8000 and most preferably about 4000.
Suds suppressing system
The detergent compositions of the invention may comprise a suds suppressing system. Where present such a sytem is found at a level of from 0.01% to 15%, preferably from 0.05% to 10%, most preferably from 0.1 % to 5 % by weight of the composition.
Suitable suds suppressing systems for use herein may comprise essentially any known antifoam compound, including, for example silicone antifoam compounds and 2-alkyl alcanol antifoam compounds.
By antifoam compound it is meant herein any compound or mixtures of compounds which act such as to depress the foaming or sudsing produced by a solution of a detergent composition, particularly in the presence of agitation of that solution.
Particularly preferred antifoam compounds for use herein are silicone antifoam compounds defined herein as any antifoam compound including a silicone component. Such silicone antifoam compounds also typically contain a silica component. The term "silicone" as used herein, and in general throughout the industry, encompasses a variety of relatively high molecular weight polymers containing siloxane units and hydrocarbyl group of various types. Preferred silicone antifoam compounds are the s iloxane s, particularly the polydimethylsiloxanes having trimethylsilyl end blocking units.
Other suitable antifoam compounds include the monocarboxylic fatty acids and soluble salts thereof. These materials are described in US
Patent 2,954,347, issued September 27, 1960 to Wayne St. John. The monocarboxylic fatty acids, and salts thereof, for use as suds suppressor typically have hydrocarbyl chains of 10 to 24 carbon atoms, preferably 12 to 18 carbon atoms. Suitable salts include the alkali metal salts such as sodium, potassium, and lithium salts, and ammonium and alkanolammonium salts.
Other suitable antifoam compounds include, for example, high molecular weight fatty esters (e.g. fatty acid triglycerides), fatty acid esters of monovalent alcohols, aliphatic C1g-C40 ketones (e.g. stearone) Nalkylated amino triazines such as tri- to hexa-alkylmelamines or di- to tetra alkyldiamine chlortriazines formed as products of cyanuric chloride with two or three moles of a primary or secondary amine containing 1 to 24 carbon atoms, propylene oxide, bis stearic acid amide and monostearyl di-alkali metal (e.g. sodium, potassium, lithium) phosphates and phosphate esters.
A preferred suds suppressing system comprises (a) antifoam compound, preferably silicone antifoam compound, most
preferably a silicone antifoam compound comprising in combination
(i) polydimethyl siloxane, at a level of from 50% to 99%,
preferably 75 % to 95 % by weight of the silicone antifoam
compound; and
(ii) silica, at a level of from 1 % to 50%, preferably 5 % to 25 % by weight of the silicone/silica antifoam compound; wherein said silica/silicone antifoam compound is incorporated at a level of from 5% to 50%, preferably 10% to 40% by weight; (b) a dispersant compound, most preferably comprising a silicone
glycol rake copolymer with a polyoxyalkylene content of 72-78 %
and an ethylene oxide to propylene oxide ratio of from 1:0.9 to
1:1.1, at a level of from 0.5% to 10%, preferably 1% to 10% by
weight; a particularly preferred silicone glycol rake copolymer of
this type is DC0544, commercially available from DOW Corning
under the tradename DCO544; (c) an inert carrier fluid compound, most preferably comprising a C 16- C18 ethoxylated alcohol with a degree of ethoxylation of from 5 to
50, preferably 8 to 15, at a level of from 5% to 80%, preferably
10% to 70SO, by weight;
A highly preferred particulate suds suppressing system is described in EP A-0210731 and comprises a silicone antifoam compound and an organic
carrier material having a melting point in the range 50"C to 85 C, wherein the organic carrier material comprises a monoester of glycerol
and a fatty acid having a carbon chain containing from 12 to 20 carbon
atoms. EP-A-0210721 discloses other preferred particulate suds
suppressing systems wherein the organic carrier material is a fatty acid or
alcohol having a carbon chain containing from 12 to 20 carbon atoms, or
a mixture thereof, with a melting point of from 45"C to 80"C.
Clay softening system
The detergent compositions may contain a clay softening system
comprising a clay mineral compound and optionally a clay flocculating
agent.
The clay mineral compound is preferably a smectite clay compound.
Smectite clays are disclosed in the US Patents No.s 3,862,058,
3,948,790, 3,954,632 and 4,062,647. European Patents No.s EP-A 299,575 and EP-A-313,146 in the name of the Procter and Gamble
Company describe suitable organic polymeric clay flocculating agents.
Polymeric dye transfer inhibiting agents
The detergent compositions herein may also comprise from 0.01 % to 10%, preferably from 0.05 % to 0.5 % by weight of polymeric dye transfer inhibiting agents.
The polymeric dye transfer inhibiting agents are preferably selected from polyamine N-oxide polymers, copolymers of N-vinylpyrrolidone and Nvinylimidazole, polyvinylpyrrolidonepolymers or combinations thereof.
a) Polvamine N-oxide polymers
Polyamine N-oxide polymers suitable for use herein contain units having the following structure formula
wherein P is a polymerisable unit, and Ais
-O-, -S-, -N-; x is O or 1;
R are aliphatic, ethoxylated aliphatics, aromatic, heterocyclic or alicyclic groups or any combination thereof whereto the nitrogen of the N-O group can be attached or wherein the nitrogen of the N-O group is part of these groups.
The N-O group can be represented by the following general structures
wherein R, R2, and R3 are aliphatic groups, aromatic, heterocyclic or alicyclic groups or combinations thereof, x or/and y or/and z is 0 or 1 and wherein the nitrogen of the N-O group can be attached or wherein the nitrogen of the N-O group forms part of these groups. The N-O group can be part of the polymerisable unit (P) or can be attached to the polymeric backbone or a combination of both.
Suitable polyamine N-oxides wherein the N-O group forms part of the polymerisable unit comprise polyamine N-oxides wherein R is selected from aliphatic, aromatic, alicyclic or heterocyclic groups. One class of said polyamine N-oxides comprises the group of polyamine N-oxides wherein the nitrogen of the N-O group forms part of the R-group.
Preferred polyamine N-oxides are those wherein R is a heterocyclic group such as pyrridine, pyrrole, imidazole, pyrrolidine, piperidine, quinoline, acridine and derivatives thereof.
Other suitable polyamine N-oxides are the polyamine oxides whereto the
N-O group is attached to the polymerisable unit. A preferred class of these polyamine N-oxides comprises the polyamine N-oxides having the general formula (I) wherein R is an aromatic,heterocyclic or alicyclic groups wherein the nitrogen of the N-O functional group is part of said R group. Examples of these classes are polyamine oxides wherein R is a heterocyclic compound such as pyrridine, pyrrole, imidazole and derivatives thereof.
The polyamine N-oxides can be obtained in almost any degree of polymerisation. The degree of polymerisation is not critical provided the material has the desired water-solubility and dye-suspending power.
Typically, the average molecular weight is within the range of 500 to 1000,000.
b) Copolymers of N-vinylpyrrolidone and N-vinylimidazole
Suitable herein are coploymers of N-vinylimidazole and Nvinylpyrrolidone having an average molecular weight range of from 5,000 to 50,000. The preferred copolymers have a molar ratio of Nvinylimidazole to N-vinylpyrrolidone from 1 to 0.2.
c) Polyvinylpyrrolidone The detergent compositions herein may also utilize polyvinylpyrrolidone ("PVP") having an average molecular weight of from 2,500 to 400,000.
Suitable polyvinylpyrrolidones are commercially available from ISP
Corporation, New York, NY and Montreal, Canada under the product names PVP K-15 (viscosity molecular weight of 10,000), PVP K-30 (average molecular weight of 40,000), PVP K-60 (average molecular weight of 160,000), and PVP K-90 (average molecular weight of 360,000). PVP K-15 is also available from ISP Corporation. Other suitable polyvinylpyrrolidones which are commercially available from
BASF Cooperation include Sokalan HP 165 and Sokalan HP 12.
d) Polyvinyloxazolidone The detergent compositions herein may also utilize polyvinyloxazolidones as polymeric dye transfer inhibiting agents. Said polyvinyloxazolidones have an average molecular weight of from 2,500 to 400,000.
e) Polyvinylimidazole
The detergent compositions herein may also utilize polyvinylimidazole as polymeric dye transfer inhibiting agent. Said polyvinylimidazoles preferably have an average molecular weight of from 2,500 to 400,000.
Optical brightener
The detergent compositions herein also optionally contain from about 0.005 % to 5 % by weight of certain types of hydrophilic optical brighteners.
Hydrophilic optical brighteners useful herein include those having the structural formula:
wherein R1 is selected from anilino, N-2-bis-hydroxyethyl and NH-2hydroxyethyl; R2 is selected from N-2-bis-hydroxyethyl, N-2hydroxyethyl-N-methylamino, morphilino, chloro and amino; and M is a salt-forming cation such as sodium or potassium.
When in the above formula, R1 is anilino, R2 is N-2-bis-hydroxyethyl and M is a cation such as sodium, the brightener is 4,4' ,-bis[(4-anilino-6- (N-2-bis-hydroxyethyl) -s -triazine-2-yl)amino] -2,2' -stilbenedisulfonic acid and disodium salt. This particular brightener species is commercially marketed under the tradename Tinopal-UNPA-GX by Ciba-Geigy
Corporation. Tinopal-UNPA-GX is the preferred hydrophilic optical brightener useful in the detergent compositions herein.
When in the above formula, R1 is anilino, R2 is N-2-hydroxyethyl-N-2methylamino and M is a cation such as sodium, the brightener is 4,4'bis [(4-anilino-6-(N-2-hydroxyethyl-N-methylamino)-s-triazine-2- yl)amino]2,2'-stilbenedisulfonic acid disodium salt. This particular brightener species is commercially marketed under the tradename Tinopal 5BM-GX by Ciba-Geigy Corporation.
When in the above formula, R1 is anilino, R2 is morphilino and M is a cation such as sodium, the brightener is 4,4'-bis[(4-anilino-6-morphilino- s-triazine-2-yl)amino] 2,2 -stilbenedisulfonic acid, sodium salt. This particular brightener species is commercially marketed under the tradename Tinopal AMS-GX by Ciba Geigy Corporation.
Cationic fabric softening agents
Cationic fabric softening agents can also be incorporated into compositions in accordance with the present invention. Suitable cationic fabric softening agents include the water insoluble tertiary amines or dilong chain amide materials as disclosed in GB-A-1 514 276 and EP-B-0 011 340.
Cationic fabric softening agents are typically incorporated at total levels of from 0.5% to 15% by weight, normally from 1% to 5% a/o by weight.
Other optional ingredients
Other optional ingredients suitable for inclusion in the compositions of the invention include perfumes, colours and filler salts, with sodium sulfate being a preferred filler salt.
pH of the compositions
The present compositions preferably have a pH measured as a 1% solution in distilled water of at least 10.0, preferably from 10.0 to 12.5, most preferably from 10.5 to 12.0.
Form of the compositions
The compositions in accordance with the invention can take a variety of physical forms including granular, tablet forms. The compositions are particularly the so-called concentrated granular detergent compositions adapted to be added to a washing machine by means of a dispensing device placed in the machine drum with the soiled fabric load.
The mean particle size of the components of granular compositions in accordance with the invention should preferably be such that no more that 5 % of particles are greater than 1 .7mm in diameter and not more than 5 % of particles are less than 0. 15mm in diameter.
The term mean particle size as defined herein is calculated by sieving a sample of the composition into a number of fractions (typically 5 fractions) on a series of Tyler sieves. The weight fractions thereby obtained are plotted against the aperture size of the sieves. The mean particle size is taken to be the aperture size through which 50% by weight of the sample would pass.
Density of the detergent composition is measured by means of a simple funnel and cup device consisting of a conical funnel moulded rigidly on a base and provided with a flap valve at its lower extremity to allow the contents of the funnel to be emptied into an axially aligned cylindrical cup disposed below the funnel. The funnel is 130 mm high and has internal diameters of 130 mm and 40 mm at its respective upper and lower extremities. It is mounted so that the lower extremity is 140 mm above the upper surface of the base. The cup has an overall height of 90 mm, an internal height of 87 mm and an internal diameter of 84 mm. Its nominal volume is 500 ml.
To carry out a measurement, the funnel is filled with powder by hand pouring, the flap valve is opened and powder allowed to overfill the cup.
The filled cup is removed from the frame and excess powder removed from the cup by passing a straight edged implement eg; a knife, across its upper edge. The filled cup is then weighed and the value obtained for the weight of powder doubled to provide a bulk density in g/litre.
Replicate measurements are made as required.
Agglomerate particles
Components used herein in granular compositions may be in the form of an agglomerate particle, which may take the form of flakes, prills, marumes, noodles, ribbons, but preferably take the form of granules. The most preferred way to process the particles is by agglomerating powders (e.g. aluminosilicate, carbonate) with high active pastes and to control the particle size of the resultant agglomerates within specified limits. Such a process involves mixing an effective amount of powder with a high active paste in one or more agglomerators such as a pan agglomerator, a Zblade mixer or more preferably an in-line mixer such as those manufactured by Schugi (Holland) BV, 29 Chroomstraat 8211 AS,
Lelystad, Netherlands, and Gebruder Lodige Maschinenbau GmbH, D4790 Paderborn 1, Elsenerstrasse 7-9, Postfach 2050, Germany. Most preferably a high shear mixer is used, such as a Lodige CB (Trade
Name).
A high active paste comprising from 50% by weight to 95 % by weight, preferably 70% by weight to 85 % by weight of surfactant is typically used. The paste may be pumped into the agglomerator at a temperature high enough to maintain a pumpable viscosity, but low enough to avoid degradation of the surfactant used. An operating temperature of the paste of 50"C to 80"C is typical.
Laundry washing method
Machine laundry methods herein typically comprise treating soiled laundry with an aqueous wash solution in a washing machine having dissolved or dispensed therein an effective amount of a machine laundry detergent composition in accord with the invention. By an effective amount of the detergent composition it is meant from 40g to 300g of product dissolved or dispersed in a wash solution of volume from 5 to 65 litres, as are typical product dosages and wash solution volumes commonly employed in conventional machine laundry methods.
In a preferred use aspect a dispensing device is employed in the washing method. The dispensing device is charged with the detergent product, and is used to introduce the product directly into the drum of the washing machine before the commencement of the wash cycle. Its volume capacity should be such as to be able to contain sufficient detergent product as would normally be used in the washing method.
Once the washing machine has been loaded with laundry the dispensing device containing the detergent product is placed inside the drum. At the commencement of the wash cycle of the washing machine water is introduced into the drum and the drum periodically rotates. The design of the dispensing device should be such that it permits containment of the dry detergent product but then allows release of this product during the wash cycle in response to its agitation as the drum rotates and also as a result of its contact with the wash water.
To allow for release of the detergent product during the wash the device may possess a number of openings through which the product may pass.
Alternatively, the device may be made of a material which is permeable to liquid but impermeable to the solid product, which will allow release of dissolved product. Preferably, the detergent product will be rapidly released at the start of the wash cycle thereby providing transient localised high concentrations of product in the drum of the washing machine at this stage of the wash cycle.
Preferred dispensing devices are reusable and are designed in such a way that container integrity is maintained in both the dry state and during the wash cycle. Especially preferred dispensing devices for use with the composition of the invention have been described in the following patents;
GB-B-2, 157, 717, GB-B-2, 157, 718, EP-A-0201376, EP-A-0288345 and EP-A-0288346. An article by J.Bland published in Manufacturing
Chemist, November 1989, pages 4146 also describes especially preferred dispensing devices for use with granular laundry products which are of a type commonly know as the "granulette". Another preferred dispensing device for use with the compositions of this invention is disclosed in PCT
Patent Application No. WO94/11562.
Especially preferred dispensing devices are disclosed in European Patent
Application Publication Nos. 0343069 & 0343070. The latter Application discloses a device comprising a flexible sheath in the form of a bag extending from a support ring defining an orifice, the orifice being adapted to admit to the bag sufficient product for one washing cycle in a washing process. A portion of the washing medium flows through the orifice into the bag, dissolves the product, and the solution then passes outwardly through the orifice into the washing medium. The support ring is provided with a masking arrangemnt to prevent egress of wetted, undissolved, product, this arrangement typically comprising radially extending walls extending from a central boss in a spoked wheel configuration, or a similar structure in which the walls have a helical form.
Alternatively, the dispensing device may be a flexible container, such as a bag or pouch. The bag may be of fibrous construction coated with a water impermeable protective material so as to retain the contents, such as is disclosed in European published Patent Application No. 0018678.
Alternatively it may be formed of a water-insoluble synthetic polymeric material provided with an edge seal or closure designed to rupture in aqueous media as disclosed in European published Patent Application
Nos. 0011500,0011501, 0011502, and 0011968. A convenient form of water frangible closure comprises a water soluble adhesive disposed along and sealing one edge of a pouch formed of a water impermeable polymeric film such as polyethylene or polypropylene.
Packaging for the compositions
Commercially marketed executions of the bleaching compositions can be packaged in any suitable container including those constructed from paper, cardboard, plastic materials and any suitable laminates. A preferred packaging execution is described in European Application No.
94921505.7.
Abbreviations used in Examples
In the detergent compositions, the abbreviated component identifications have the following meanings:
LAS . Sodium linear C 12 alkyl benzene sulfonate
Nonionic 45E7 : A C14-15 predominantly linear primary alcohol
condensed with an average of 7 moles of
ethylene oxide
QAS R2.N+(CH3)3 with R2 = C12 - C14
STPP Anhydrous sodium tripolyphosphate
Carbonate Anhydrous sodium carbonate with a particle size
between 200zm and 900pm Silicate Amorphous Sodium Silicate (SiO2:Na2O; 2.0
ratio)
Sodium sulfate : Anhydrous sodium sulfate
MA/AA Copolymer of 1:4 maleic/acrylic acid, average
molecular weight about 70,000.
CMC Sodium carboxymethyl cellulose
Protease Proteolytic enzyme of activity 4KNPU/g sold by
NOVO Industries A/S under the tradename
Savinase
Alcalase Proteolytic enzyme of activity 3AU/g sold by
NOVO Industries A/S
Cellulase Cellulytic enzyme of activity 1000 CEVU/g sold
by NOVO Industries A/S under the tradename C arezyme Amylase Amylolytic enzyme of activity 60KNU/g sold by
NOVO Industries A/S under the tradename
Termamyl 60T
Lipase Lipolytic enzyme of activity 100kLU/g sold by
NOVO Industries A/S under the tradename
Lipolase
PB 1 Anhydrous sodium perborate bleach of
nominal formula NaB02.H2O2 TAED Tetraacetylethylenediamine 480N Random copolymer of 3:7 acrylic/methacrylic
acid, average molecular weight about 3,500
DTPA(A) . Diethylene triamine pentaacetic acid Photoactivated : Sulfonated Zinc Phthlocyanine encapsulated in bleach dextrin soluble polymer
SRP Sulfobenzoyl end capped esters with oxyethylene
oxy and terephtaloyl backbone
Silicone antifoam: Polydimethylsiloxane foam controller with
siloxane-oxyalkylene copolymer as dispersing
agent with a ratio of said foam controller to said
dispersing agent of 10:1 to 100:1.
In the following Examples all levels are quoted as % by weight of the composition:
Example 1
Compositions B to D were prepared with accord to the present invention.
Composition A is a comparative composition known in the art and X is a nil-sulphate composition.
A B C D X Blown Powder LAS 19.3 21.5 22.4 25.3 31.29 STPP 21.0 21.8. 24.3 27.5 34.05 Silicate 8.0 8.9 9.2 10.4 12.97 Sulphate 38.2 32.1 28.5 19.1 Dry Add Carbonate 5.0 5.4 5.7 6.5 8.11 Perfume 0.06 0.07 0.07 0.08 0.10 or anic/inor anic ratio 0.286 0.343 0.362 0.444 0.665 CMM % 34 35 36 39 43 Density g/L 360 ~ 320 310 300 260 Example 2
Compositions F to I were prepared with accord to the present invention.
Composition E is a comparative composition known in the art and Y represents a nil-sulphate composition.
EFGH I Y Blown Powder LAS 19.3 20.4 21.3 23.4 25.38 27.41 QAS 0.63 0.65 0.67 0.70 0.82 0.89 STPP 25.0 27.1 27.6 30.3 32.88 35.51 Silicate 7.6 7.9 8.3 9.1 9.9 10.79 Sulphate 29.4 25.6 22.0 14.7 7.36 - DTPA(A) 0.21 0.23 0.23 0.25 0.27 0.29 MA/AA 1.0 1.1 1.1 1.2 1.31 1.4 Dry Add Carbonate 5.0 5.3 5.5 6.05 6.57 7.1 Protease 0.6 0.6 0.6 0.72 0.78 0.8 Lipase 0.15 0.16 0.17 0.18 0.19 0.21 Amylase 0.36 0.38 0.39 0.40 0.47 0.51 SRP 0.14 0.14 0.15 0.16 0.18 0.19 organic/inorganic 0.338 0.369 0.381 0.476 0.554 0.648 ratio CMM % 34 35 35 37 40 42 Density g/L 400 370 360 340 320 300 Example 3
Compositions K and L were prepared with accord to the present invention. Composition J is a comparative composition known in the art and Z represents a nil-sulphate composition.
J K L Z Blown Powder LAS 6.65 7.38 7.74 8.11 Silicate 6.7 7.4 7.80 8.17 MA/AA 0.95 1.05 1.11 1.15 DTPA(A) 0.27 0.28 0.31 0.33 STPP 25.7 28.53 29,95 31.36 Sulphate 19.9 8.9 4.49 Nonionic 45E7 4.7 5.27 5.53 5.79 Silicone antifoam 0.34 0.37 0.39 0.42 480N 0.04 0.04 0.05 0.05 Dry Add Carbonate 11.4 12.65 13.28 13.91 Protease 0.47 0.53 0.54 0.57 Lipase 0.1 0.116 0.12 0.122 Amylase 0.38 0.42 0.44 0.46 SRP 0.1 0.111 0.12 0.122 Cellulase 0.08 0.09 0.09 0.09 PB1 10.45 11.60 12.17 12.75 TAED 1.28 1.42 1.49 1.56 Photoactivated 0.003 0.003 0.003 0.003 organic/inorganic ratio 0.249 0.354 0.358 0.401 CMM % 34 ~ 34 34 34 Density g/L 500 470 455 ~ 440 Measurement of Caking
The compositions prepared by the process of the present invention are less predisposed to caking than other reduced and nil-sulphate compositions previously documented. Caking potential is measured by a standard test procedure for measuring cake strength. In general terms the cake strength test is a measure of the force required to break a detergent composition cake pre-packed at a specific pressure. The 'stickier' the detergent components, the greater the force required to break the cake.
The cake strength measuring equipment consists essentially of a solid perspex cylinder, with a polished surface (diameter 6.35cm, length 15.90cm), a hollow perspex sleeve with a polished inner surface (inner diameter 6.35cm, wall thickness 1.5cm, length 15.25cm), a perspex disc lid (diameter 11.5cm and thickness 0.65cm), a 5 Kg weight and a force gauge.
The sleeve and cylinder, the latter fitted inside the former, are placed vertically on a flat surface. The cylinder/sleeve is filled with detergent composition which has been stored at 350C for 12 hours. The detergent composition in the cylinder/sleeve is levelled using a straight edged knife and the lid fitted on the top of the detergent. The 5 Kg weight is then placed on the lid, such that the weight provides an even pressure across the surface of the lid. The weight is left to compress the detergent for 2 minutes. After 2 minutes, the weight is removed and the sleeve slid downward, leaving a cake of detergent. The force gauge is then directed to the centre of the lid and the force required to break the cake is noted.
The following scale is representative of consumer perception.
Cake Strength / lbs Consumer Perception
0 excellent
1 very good
2 good
3 satisfactory
4/5 poor
6/7 unacceptable
Table 1. represents cake strength data produced for the compositions described in Example 2 (compositions E, F, G, H, I and Y)
E F G H I Y Cake Strength / lbs 0 0 0 1 2 6 CMM % 34 35 35 37 40 42 Table 1.
It can be seen from the data described in table 1, that the compositions of the present invention have reduced potential for caking.
Claims (12)
1. A process for preparing a detergent composition, said process comprising spray drying a slurry of organic and inorganic material wherein the ratio of organic to inorganic material is from 0.34 to 0.64, and said slurry having a moisture content of between 25 % and 50 % .
2. A process according to Claim 1 wherein the organic to inorganic ratio is from 0.36 to 0.48.
3. A process according to either of Claims 1 or 2 wherein the slurry has a moisture content of between 34 % and 43 % .
4. A process according to any of Claims 1 to 3 wherein air is injected into the slurry of organic and inorganic material.
5. A process according to any of Claims 1 to 4 wherein the organic material is an organic surfactant.
6. A process according to Claim 5 wherein the organic surfactant is an anionic, cationic or amphoteric surfactant.
7. A process according to either of Claims 5 or 6 wherein the organic surfactant is linear alkylbenzene sulphonate.
8. A process according to any of Claims 1 to 7 wherein the inorganic material is selected from the group consisting of phosphate, carbonate, aluminosilicate, crystalline layered silicate, citrate, alkali metal and/or alkali earth metal silicate and sulphate or mixtures thereof.
9. A process according to Claim 8 wherein the ratio of organic to inorganic material is altered by addition or deletion of alkali metal and/or alkali earth metal sulphate.
10. A detergent composition prepared by the process according to any of of Claims 1 to 9.
11. A detergent composition according to Claim 10 having density of less than 599 g/l.
12. A detergent composition according to Claim 10 having density of 400g/l or less.
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB9622272A GB2318584A (en) | 1996-10-25 | 1996-10-25 | Process for preparing detergent compositions by spray drying |
BR9712650-0A BR9712650A (en) | 1996-10-25 | 1997-10-14 | Detergent composition |
PCT/US1997/018424 WO1998018895A1 (en) | 1996-10-25 | 1997-10-14 | Detergent compositions |
CA002269475A CA2269475C (en) | 1996-10-25 | 1997-10-14 | Detergent compositions |
EP97910912A EP0934395A4 (en) | 1996-10-25 | 1997-10-14 | Detergent compositions |
ARP970104934 AR010029A1 (en) | 1996-10-25 | 1997-10-24 | PROCESS TO PREPARE A DETERGENT COMPOSITION AND SUCH DETERGENT COMPOSITION |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB9622272A GB2318584A (en) | 1996-10-25 | 1996-10-25 | Process for preparing detergent compositions by spray drying |
Publications (2)
Publication Number | Publication Date |
---|---|
GB9622272D0 GB9622272D0 (en) | 1996-12-18 |
GB2318584A true GB2318584A (en) | 1998-04-29 |
Family
ID=10801967
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB9622272A Withdrawn GB2318584A (en) | 1996-10-25 | 1996-10-25 | Process for preparing detergent compositions by spray drying |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP0934395A4 (en) |
AR (1) | AR010029A1 (en) |
BR (1) | BR9712650A (en) |
CA (1) | CA2269475C (en) |
GB (1) | GB2318584A (en) |
WO (1) | WO1998018895A1 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ATE501243T1 (en) * | 2006-10-16 | 2011-03-15 | Procter & Gamble | SPRAY DRYING METHOD FOR PRODUCING SPRAY DRIED, HIGHLY WATER SOLUBLE, LOW DENSITY AND LOW BUILDER CONTENT DETERGENTS. |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3709837A (en) * | 1970-12-30 | 1973-01-09 | Philadelphia Quartz Co | Spray dried detergents containing sodium-potassium double silicate |
US3801511A (en) * | 1972-04-17 | 1974-04-02 | Procter & Gamble | Spray-dried detergent composition |
US4344871A (en) * | 1981-03-23 | 1982-08-17 | The Procter & Gamble Company | Spray-dried aluminosilicate detergents containing silicate and metaborate |
US4478735A (en) * | 1981-05-20 | 1984-10-23 | Lion Corporation | Process for producing granular detergent composition |
EP0349199A1 (en) * | 1988-06-29 | 1990-01-03 | The Procter & Gamble Company | Two stage drying of detergent compositions |
EP0242138B1 (en) * | 1986-04-14 | 1991-09-11 | Unilever Plc | Process for the preparation of detergent powders |
WO1993003131A1 (en) * | 1991-07-30 | 1993-02-18 | Henkel Kommanditgesellschaft Auf Aktien | Anionic-surfactant preparation in powder form |
WO1993012216A1 (en) * | 1991-12-17 | 1993-06-24 | Henkel Kommanditgesellschaft Auf Aktien | GRANULATE CONTAINING α SULPHO-FATTY ACID ALKYL ESTER |
WO1994005767A1 (en) * | 1992-09-08 | 1994-03-17 | Unilever Plc | Detergent composition and process for its production |
WO1996002621A1 (en) * | 1994-07-19 | 1996-02-01 | Crosfield Limited | Method for preparing co-granules, co-granules thus obtained and use thereof as a component in detergent compositions |
Family Cites Families (13)
Publication number | Priority date | Publication date | Assignee | Title |
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US4006110A (en) * | 1971-11-30 | 1977-02-01 | Colgate-Palmolive Company | Manufacture of free-flowing particulate heavy duty synthetic detergent composition |
JPS5254709A (en) * | 1975-10-31 | 1977-05-04 | Lion Corp | Multi-stage spray drying method |
US4129526A (en) * | 1977-07-14 | 1978-12-12 | The Lion Fat & Oil Co., Ltd. | Granular detergent compositions and a process for producing same |
US4180485A (en) * | 1977-11-02 | 1979-12-25 | The Procter & Gamble Company | Spray-dried detergent compositions |
GB2020687B (en) * | 1978-05-11 | 1982-09-22 | Unilever Ltd | Washing powdwe |
US4552681A (en) * | 1983-12-10 | 1985-11-12 | Henkel Kommanditgesellschaft Auf Aktien | Granular, free-flowing detergent component and method for its production |
GB8502032D0 (en) * | 1985-01-28 | 1985-02-27 | Unilever Plc | Detergent powder |
DE3833648A1 (en) * | 1988-10-04 | 1990-04-05 | Henkel Kgaa | METHOD FOR PRODUCING PARTICLE-DETERGENT DETERGENTS |
GB2231579A (en) * | 1989-05-09 | 1990-11-21 | Unilever Plc | Spray-dried detergent |
DE4139551A1 (en) * | 1991-11-30 | 1993-06-03 | Henkel Kgaa | POWDERED SURFACE BLEND |
DE4213036A1 (en) * | 1992-04-21 | 1993-10-28 | Henkel Kgaa | Stable, free-flowing granulate of alkaline cleaning additive - contg. (meth)acrylic] acid (co)polymer, sodium silicate, sodium carbonate or sodium sulphate, sequestering agent and water |
DE4216775A1 (en) * | 1992-05-21 | 1993-11-25 | Henkel Kgaa | Powdery surfactant mixture |
DE4310671A1 (en) * | 1993-04-01 | 1994-10-06 | Henkel Kgaa | Granules containing alpha-sulfofatty acid alkyl ester |
-
1996
- 1996-10-25 GB GB9622272A patent/GB2318584A/en not_active Withdrawn
-
1997
- 1997-10-14 BR BR9712650-0A patent/BR9712650A/en not_active Application Discontinuation
- 1997-10-14 EP EP97910912A patent/EP0934395A4/en not_active Withdrawn
- 1997-10-14 CA CA002269475A patent/CA2269475C/en not_active Expired - Fee Related
- 1997-10-14 WO PCT/US1997/018424 patent/WO1998018895A1/en not_active Application Discontinuation
- 1997-10-24 AR ARP970104934 patent/AR010029A1/en not_active Application Discontinuation
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3709837A (en) * | 1970-12-30 | 1973-01-09 | Philadelphia Quartz Co | Spray dried detergents containing sodium-potassium double silicate |
US3801511A (en) * | 1972-04-17 | 1974-04-02 | Procter & Gamble | Spray-dried detergent composition |
US4344871A (en) * | 1981-03-23 | 1982-08-17 | The Procter & Gamble Company | Spray-dried aluminosilicate detergents containing silicate and metaborate |
US4478735A (en) * | 1981-05-20 | 1984-10-23 | Lion Corporation | Process for producing granular detergent composition |
EP0242138B1 (en) * | 1986-04-14 | 1991-09-11 | Unilever Plc | Process for the preparation of detergent powders |
EP0349199A1 (en) * | 1988-06-29 | 1990-01-03 | The Procter & Gamble Company | Two stage drying of detergent compositions |
WO1993003131A1 (en) * | 1991-07-30 | 1993-02-18 | Henkel Kommanditgesellschaft Auf Aktien | Anionic-surfactant preparation in powder form |
WO1993012216A1 (en) * | 1991-12-17 | 1993-06-24 | Henkel Kommanditgesellschaft Auf Aktien | GRANULATE CONTAINING α SULPHO-FATTY ACID ALKYL ESTER |
WO1994005767A1 (en) * | 1992-09-08 | 1994-03-17 | Unilever Plc | Detergent composition and process for its production |
WO1996002621A1 (en) * | 1994-07-19 | 1996-02-01 | Crosfield Limited | Method for preparing co-granules, co-granules thus obtained and use thereof as a component in detergent compositions |
Also Published As
Publication number | Publication date |
---|---|
CA2269475A1 (en) | 1998-05-07 |
GB9622272D0 (en) | 1996-12-18 |
AR010029A1 (en) | 2000-05-17 |
WO1998018895A1 (en) | 1998-05-07 |
BR9712650A (en) | 2000-10-24 |
CA2269475C (en) | 2002-12-24 |
EP0934395A4 (en) | 2000-02-23 |
EP0934395A1 (en) | 1999-08-11 |
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Legal Events
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WAP | Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1) |