EP4341368A1 - Process for preparing a spray dried detergent particle - Google Patents
Process for preparing a spray dried detergent particleInfo
- Publication number
- EP4341368A1 EP4341368A1 EP22729211.7A EP22729211A EP4341368A1 EP 4341368 A1 EP4341368 A1 EP 4341368A1 EP 22729211 A EP22729211 A EP 22729211A EP 4341368 A1 EP4341368 A1 EP 4341368A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- salt
- alkaline earth
- spray
- earth metal
- silicate
- 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.)
- Pending
Links
- 239000003599 detergent Substances 0.000 title claims abstract description 114
- 239000002245 particle Substances 0.000 title claims abstract description 109
- 239000007921 spray Substances 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 130
- -1 alkaline earth metal salt Chemical class 0.000 claims abstract description 82
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 77
- 239000004094 surface-active agent Substances 0.000 claims abstract description 68
- 239000002002 slurry Substances 0.000 claims abstract description 63
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 44
- 150000004760 silicates Chemical class 0.000 claims abstract description 42
- 238000001694 spray drying Methods 0.000 claims abstract description 35
- 239000000945 filler Substances 0.000 claims abstract description 32
- 238000011065 in-situ storage Methods 0.000 claims abstract description 32
- 150000003839 salts Chemical class 0.000 claims abstract description 30
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 26
- 239000010457 zeolite Substances 0.000 claims abstract description 14
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract 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 abstract description 13
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 6
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 5
- 239000010452 phosphate Substances 0.000 claims abstract description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 40
- 239000003945 anionic surfactant Substances 0.000 claims description 37
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 30
- 229920000642 polymer Polymers 0.000 claims description 28
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 21
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 19
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000004115 Sodium Silicate Substances 0.000 claims description 17
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 17
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 17
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 15
- 239000004615 ingredient Substances 0.000 claims description 15
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 15
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 15
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- 102000004190 Enzymes Human genes 0.000 claims description 10
- 108090000790 Enzymes Proteins 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 10
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims description 9
- 239000000975 dye Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 150000001860 citric acid derivatives Chemical class 0.000 claims description 7
- 229910021532 Calcite Inorganic materials 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 239000010459 dolomite Substances 0.000 claims description 6
- 229910000514 dolomite Inorganic materials 0.000 claims description 6
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 6
- 239000001095 magnesium carbonate Substances 0.000 claims description 6
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 6
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 4
- 239000006260 foam Substances 0.000 claims description 4
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 4
- 235000011147 magnesium chloride Nutrition 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 4
- 239000000049 pigment Substances 0.000 claims description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 235000011148 calcium chloride Nutrition 0.000 claims description 3
- HHSPVTKDOHQBKF-UHFFFAOYSA-J calcium;magnesium;dicarbonate Chemical compound [Mg+2].[Ca+2].[O-]C([O-])=O.[O-]C([O-])=O HHSPVTKDOHQBKF-UHFFFAOYSA-J 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 150000004679 hydroxides Chemical class 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 239000001175 calcium sulphate Substances 0.000 claims description 2
- 235000011132 calcium sulphate Nutrition 0.000 claims description 2
- 239000002304 perfume Substances 0.000 claims description 2
- 239000003352 sequestering agent Substances 0.000 claims description 2
- 229940077388 benzenesulfonate Drugs 0.000 claims 1
- 230000000007 visual effect Effects 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 32
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 8
- 238000004140 cleaning Methods 0.000 abstract description 6
- 125000000217 alkyl group Chemical group 0.000 description 16
- 235000017550 sodium carbonate Nutrition 0.000 description 15
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 14
- 238000003860 storage Methods 0.000 description 14
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 9
- 229940088598 enzyme Drugs 0.000 description 8
- 230000003472 neutralizing effect Effects 0.000 description 8
- 125000000129 anionic group Chemical group 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000002585 base Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 229910052938 sodium sulfate Inorganic materials 0.000 description 7
- 235000011152 sodium sulphate Nutrition 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 6
- 239000000391 magnesium silicate Substances 0.000 description 6
- 229910052919 magnesium silicate Inorganic materials 0.000 description 6
- 235000019792 magnesium silicate Nutrition 0.000 description 6
- 239000002689 soil Substances 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
- 150000008044 alkali metal hydroxides Chemical group 0.000 description 5
- 238000012669 compression test Methods 0.000 description 5
- 235000014113 dietary fatty acids Nutrition 0.000 description 5
- 239000000194 fatty acid Substances 0.000 description 5
- 229930195729 fatty acid Natural products 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 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 4
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- 150000005323 carbonate salts Chemical class 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 150000004665 fatty acids Chemical class 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 229910052816 inorganic phosphate Inorganic materials 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000000344 soap Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- YGUMVDWOQQJBGA-VAWYXSNFSA-N 5-[(4-anilino-6-morpholin-4-yl-1,3,5-triazin-2-yl)amino]-2-[(e)-2-[4-[(4-anilino-6-morpholin-4-yl-1,3,5-triazin-2-yl)amino]-2-sulfophenyl]ethenyl]benzenesulfonic acid Chemical compound C=1C=C(\C=C\C=2C(=CC(NC=3N=C(N=C(NC=4C=CC=CC=4)N=3)N3CCOCC3)=CC=2)S(O)(=O)=O)C(S(=O)(=O)O)=CC=1NC(N=C(N=1)N2CCOCC2)=NC=1NC1=CC=CC=C1 YGUMVDWOQQJBGA-VAWYXSNFSA-N 0.000 description 3
- XASDIFBXOWQKFW-UHFFFAOYSA-N [Mg+2].[Mg+2].[Mg+2].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] XASDIFBXOWQKFW-UHFFFAOYSA-N 0.000 description 3
- 238000005273 aeration Methods 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 3
- 229910052915 alkaline earth metal silicate Inorganic materials 0.000 description 3
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 3
- 159000000007 calcium salts Chemical class 0.000 description 3
- 159000000003 magnesium salts Chemical class 0.000 description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 239000005022 packaging material Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920000058 polyacrylate Polymers 0.000 description 3
- 229920005646 polycarboxylate Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000013042 solid detergent Substances 0.000 description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- CFPOJWPDQWJEMO-UHFFFAOYSA-N 2-(1,2-dicarboxyethoxy)butanedioic acid Chemical class OC(=O)CC(C(O)=O)OC(C(O)=O)CC(O)=O CFPOJWPDQWJEMO-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- LVVZBNKWTVZSIU-UHFFFAOYSA-N 2-(carboxymethoxy)propanedioic acid Chemical class OC(=O)COC(C(O)=O)C(O)=O LVVZBNKWTVZSIU-UHFFFAOYSA-N 0.000 description 2
- CNGYZEMWVAWWOB-VAWYXSNFSA-N 5-[[4-anilino-6-[bis(2-hydroxyethyl)amino]-1,3,5-triazin-2-yl]amino]-2-[(e)-2-[4-[[4-anilino-6-[bis(2-hydroxyethyl)amino]-1,3,5-triazin-2-yl]amino]-2-sulfophenyl]ethenyl]benzenesulfonic acid Chemical compound N=1C(NC=2C=C(C(\C=C\C=3C(=CC(NC=4N=C(N=C(NC=5C=CC=CC=5)N=4)N(CCO)CCO)=CC=3)S(O)(=O)=O)=CC=2)S(O)(=O)=O)=NC(N(CCO)CCO)=NC=1NC1=CC=CC=C1 CNGYZEMWVAWWOB-VAWYXSNFSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- 108010065511 Amylases Proteins 0.000 description 2
- 102000013142 Amylases Human genes 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 102100032487 Beta-mannosidase Human genes 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- OCUCCJIRFHNWBP-IYEMJOQQSA-L Copper gluconate Chemical class [Cu+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 OCUCCJIRFHNWBP-IYEMJOQQSA-L 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- 108090001060 Lipase Proteins 0.000 description 2
- 102000004882 Lipase Human genes 0.000 description 2
- 239000004367 Lipase Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- JYXGIOKAKDAARW-UHFFFAOYSA-N N-(2-hydroxyethyl)iminodiacetic acid Chemical class OCCN(CC(O)=O)CC(O)=O JYXGIOKAKDAARW-UHFFFAOYSA-N 0.000 description 2
- 108090000854 Oxidoreductases Proteins 0.000 description 2
- 102000004316 Oxidoreductases Human genes 0.000 description 2
- 108091005804 Peptidases Proteins 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- 239000004365 Protease Substances 0.000 description 2
- 229920006243 acrylic copolymer Polymers 0.000 description 2
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 2
- 150000008041 alkali metal carbonates Chemical class 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 235000019418 amylase Nutrition 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 108010055059 beta-Mannosidase Proteins 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007844 bleaching agent Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 2
- 235000011180 diphosphates Nutrition 0.000 description 2
- 238000007580 dry-mixing Methods 0.000 description 2
- 238000007046 ethoxylation reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 235000019421 lipase Nutrition 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229920005996 polystyrene-poly(ethylene-butylene)-polystyrene Polymers 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 235000019832 sodium triphosphate Nutrition 0.000 description 2
- 150000003890 succinate salts Chemical class 0.000 description 2
- 239000002888 zwitterionic surfactant Substances 0.000 description 2
- CIOXZGOUEYHNBF-UHFFFAOYSA-N (carboxymethoxy)succinic acid Chemical class OC(=O)COC(C(O)=O)CC(O)=O CIOXZGOUEYHNBF-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 239000004382 Amylase Substances 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 108010059892 Cellulase Proteins 0.000 description 1
- 108010084185 Cellulases Proteins 0.000 description 1
- 102000005575 Cellulases Human genes 0.000 description 1
- 108010023736 Chondroitinases and Chondroitin Lyases Proteins 0.000 description 1
- 102000011413 Chondroitinases and Chondroitin Lyases Human genes 0.000 description 1
- 101710121765 Endo-1,4-beta-xylanase Proteins 0.000 description 1
- 108090000371 Esterases Proteins 0.000 description 1
- 108010003272 Hyaluronate lyase Proteins 0.000 description 1
- 102000001974 Hyaluronidases Human genes 0.000 description 1
- 108010029541 Laccase Proteins 0.000 description 1
- 102000003820 Lipoxygenases Human genes 0.000 description 1
- 108090000128 Lipoxygenases Proteins 0.000 description 1
- 241000282320 Panthera leo Species 0.000 description 1
- 102000035195 Peptidases Human genes 0.000 description 1
- 108700020962 Peroxidase Proteins 0.000 description 1
- 102000003992 Peroxidases Human genes 0.000 description 1
- 108010064785 Phospholipases Proteins 0.000 description 1
- 102000015439 Phospholipases Human genes 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 108010059820 Polygalacturonase Proteins 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- 108091007187 Reductases Proteins 0.000 description 1
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 206010057040 Temperature intolerance Diseases 0.000 description 1
- 102000003425 Tyrosinase Human genes 0.000 description 1
- 108060008724 Tyrosinase Proteins 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000005276 aerator Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 108090000637 alpha-Amylases Proteins 0.000 description 1
- 108010084650 alpha-N-arabinofuranosidase Proteins 0.000 description 1
- 150000001414 amino alcohols Chemical class 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 229940025131 amylases Drugs 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000002752 cationic softener Substances 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000000332 coumarinyl group Chemical class O1C(=O)C(=CC2=CC=CC=C12)* 0.000 description 1
- 108010005400 cutinase Proteins 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- PMPJQLCPEQFEJW-HPKCLRQXSA-L disodium;2-[(e)-2-[4-[4-[(e)-2-(2-sulfonatophenyl)ethenyl]phenyl]phenyl]ethenyl]benzenesulfonate Chemical group [Na+].[Na+].[O-]S(=O)(=O)C1=CC=CC=C1\C=C\C1=CC=C(C=2C=CC(\C=C\C=3C(=CC=CC=3)S([O-])(=O)=O)=CC=2)C=C1 PMPJQLCPEQFEJW-HPKCLRQXSA-L 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 108010093305 exopolygalacturonase Proteins 0.000 description 1
- 239000002979 fabric softener Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000008543 heat sensitivity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 108010002430 hemicellulase Proteins 0.000 description 1
- 229960002773 hyaluronidase Drugs 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 108010059345 keratinase Proteins 0.000 description 1
- 238000004900 laundering Methods 0.000 description 1
- 108010062085 ligninase Proteins 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 108010087558 pectate lyase Proteins 0.000 description 1
- 229920001983 poloxamer Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000010349 pulsation Effects 0.000 description 1
- 150000003219 pyrazolines Chemical class 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910021647 smectite Inorganic materials 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical group O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 235000019794 sodium silicate Nutrition 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000007916 tablet composition Substances 0.000 description 1
- 108010038851 tannase Proteins 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 108010083879 xyloglucan endo(1-4)-beta-D-glucanase Proteins 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/10—Carbonates ; Bicarbonates
-
- 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
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/08—Silicates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/122—Sulfur-containing, e.g. sulfates, sulfites or gypsum
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/1233—Carbonates, e.g. calcite or dolomite
Definitions
- the present invention relates to a process for preparing a particulate, free flowing detergent particle by a slurry making and spray drying technique.
- the spray-dried particle is suitable for use as a solid laundry detergent composition, or for incorporation into a solid laundry detergent composition.
- granular laundry detergent composition is prepared by spray-drying.
- the detergent components such as surfactants and builders are mixed with around 20% to 50% by weight water to form an aqueous slurry, the aqueous slurry is maintained at temperatures ranging from 60°C to 85°C and then spray-dried in a spray-drying tower.
- Lumping and caking of the spray-dried detergent composition has been a common problem faced by the consumers. There has been a continued effort towards improving the properties of the spray dried powder.
- the consumers During use, the consumers generally store the solid laundry detergent composition close to the washing machine or the washing area. These regions are generally subjected to higher humidity. Further after opening the pouch containing the detergent composition, the consumers usually either empty the solid detergent composition into a container or store the powder along with the pouch in the container. However, during storage moisture ingress overtime into the solid detergent composition, which is either absorbed from the air, or transferred from the wet scoop used to dose the solid detergent composition.
- Such concentrated solid laundry detergent composition/spray dried detergent particle with at least 40 w.% surfactant content must also be free flowing to be dosed accurately and must retain good flow properties over extended storage life.
- US3849346 discloses a process for preparing a granular detergent composition containing particles of relatively high mechanical strength and which are essentially non-caking. The process includes the step of spray-drying a slurry comprising anionic surface-active agent, sodium tripolyphosphate, sodium silicate and magnesium sulphate to form in-situ magnesium silicate and magnesium phosphate. More recently, WO 2006/029676 A1 (Unilever) discloses a laundry detergent composition with a soluble alkali metal silicate and 0.01 wt.% to 25 wt.% alkaline earth silicate seeds. The alkaline earth silicate seeds are formed in-situ by reaction of sodium silicate and soluble alkaline earth metal salt in presence of anionic surfactant during the laundry detergent base powder processing.
- US 2009/325847 A1 discloses a process for forming a spray-dried particle which has good stability profile.
- the aqueous slurry includes 4.32 wt.% sodium carbonate and forms a spray-dried detergent particle having magnesium sulphate, 5.77 wt.% sodium carbonate and 63.43 wt.% sodium sulphate.
- US 4139486 A (Bailey John et. al., 1979) discloses a detergent composition having superior whiteness maintenance and lower undesirable residual deposits on the fabrics which composition includes orthophosphate and pyrophosphate together as builder along with the addition of magnesium silicate.
- WO 2005/037712 A1 discloses a detergent composition having a soluble carbonate salt in combination with a soluble alkali metal silicate. It discloses a method of preparing amorphous particles of silicate-based calcium salt or silicate- based magnesium salt having the step of mixing an aqueous solution of a calcium salt or magnesium salt with a soluble alkali metal silicate salt and a soluble carbonate salt.
- EP 2138565 A1 discloses a spray-drying process where an alkaline slurry is formed in a mixer, and a portion of the acid anionic detersive surfactant precursor is contacted with the alkaline slurry after the mixer and before the spray pressure nozzle to form a mixture, the mixture is then sprayed through the spray pressure nozzle into the spray-drying tower to form a spray-dried powder.
- a spray-dried detergent particle having hygroscopic fillers exhibits extended shelf life and demonstrates excellent powder properties without getting caked during use, when the spray dried detergent particle is prepared by a process where an in-situ silicate and/or a disilicate a salt of an alkaline earth metal is formed by reacting an alkali metal silicate with an alkaline earth metal salt, and the spray dried detergent particle also includes an alkali metal silicate salt along with optimum detersive surfactant content and carbonate builder, wherein the composition has no phosphate builder and preferably no zeolite builder.
- the spray dried detergent particle according to the present invention preferably incorporates optimum amounts of alkaline builders, particularly alkali metal silicates and alkali metal carbonates.
- alkaline builders particularly alkali metal silicates and alkali metal carbonates.
- a process of preparing a spray-dried detergent particle comprising the steps as described herein below.
- the first aspect of the present invention disclosed is a process of contacting an alkaline earth metal salt with an alkali metal silicate in an aqueous mixture.
- the aqueous mixture comprises a detersive surfactant.
- the alkaline earth metal salt is preferably a magnesium or a calcium salt or mixtures thereof.
- the alkaline earth metal salt may be preferably selected from calcium sulphate, magnesium sulphate, calcium chloride, magnesium chloride or mixtures thereof.
- the alkali earth metal is a magnesium salt selected from magnesium sulphate, magnesium chloride or mixtures thereof and still preferably the alkaline earth metal salt is magnesium sulphate.
- the process according to the present invention includes addition of an alkali metal silicate to the aqueous mixture.
- the alkali metal silicate is a soluble silicate.
- Soluble silicates are common ingredients in the laundry detergent compositions. Some commercial grades of silicates may contain a trace level of alkaline earth metal silicate, as contamination.
- the composition of trace materials in the water used for making an aqueous mixture having detersive surfactant may also contribute to the alkaline earth metal. However, the amount of amorphous material introduced through this impurity route will be low.
- the spray-dried detergent particle prepared according to the process of the first aspect of the present invention preferably includes 0.1 wt.% to 2.5 wt.% amorphous alkaline earth metal silicate prepared in-situ.
- the alkali metal silicate salt preferably has a weight ratio of SiC ⁇ I hO where M is an alkali metal, within the range of 1.6 to 3.3 more preferably 1.6 to 2.4, and most preferably 2.0 to 2.85.
- the alkali metal silicate salt employed is preferably in the form of an aqueous solution, generally having 30 wt.% to 45 wt.% solid content.
- the alkali metal silicate salt may be selected from the group consisting of sodium silicate, potassium silicate, sodium-potassium double silicate or mixtures thereof.
- the alkali metal silicate salt is water-soluble.
- the alkali metal silicate salt employed is sodium silicate.
- the sodium silicate has a weight ratio, SiC> 2 :Na 2 0 within the range of 1.6 to 3.3 more preferably 1.6 to 2.4, and most preferably 2.0 to 2.85.
- the amount of alkali metal silicate present in the aqueous mixture is in stoichiometric excess of the amount required for reacting with alkaline earth metal salt.
- the amount of alkali metal silicate present in the aqueous mixture is such that the spray dried detergent particle formed preferably comprises from 5 wt.% to 17 wt.% alkali metal silicate salt.
- the amount of alkali metal silicate added to the aqueous mixture is from 8 wt.% to 30 wt.% by weight of the aqueous mixture.
- the excess amount of alkali metal silicate (after the formation of the in-situ alkaline earth metal silicate) may be added into the slurry at any stage before spray-drying, more preferably after the addition of filler.
- the weight ratio between the alkali metal silicate to the alkaline earth metal salt added to the aqueous mixture is in the range from 260:1 to 5:1, preferably 24:1 to 12:1.
- Aqueous mixture is in the range from 260:1 to 5:1, preferably 24:1 to 12:1.
- the aqueous mixture comprises a detersive surfactant.
- the aqueous mixture includes a detersive surfactant.
- the detersive surfactant is preferably an anionic surfactant.
- the detersive anionic surfactant is either pre-neutralized and added into the aqueous mixture or a liquid acid form of the anionic surfactant is added to the aqueous mixture and neutralized in-situ.
- the acid form of the anionic surfactant may be partly neutralized and thereafter added into the aqueous mixture such that the remaining un-neutralized part of the liquid acid form of the anionic surfactant is neutralized in-situ in the aqueous mixture.
- Pre-neutralized surfactant is commercially available in solid form or in the form of paste.
- the detersive surfactant is added to the aqueous mixture before addition of the alkaline earth metal salt.
- the detersive surfactant is added to the aqueous mixture after addition of the alkaline earth metal salt or along with the alkaline earth metal salt.
- the partly neutralized anionic surfactant is preferably prepared by a neutralization process which involves the step of (i) mixing a liquid acid form of the anionic surfactant and a neutralizing agent to form a partially neutralized solution; preferably the neutralizing agent is an alkali metal hydroxide, wherein the amount of alkali metal hydroxide neutralizing agent is sufficient to react with a portion of liquid acid anionic surfactant precursor to form in-situ anionic surfactant salt.
- the neutralized anionic surfactant formed by neutralizing the acid form with the alkali metal hydroxide neutralizing agent contributes from 28 parts to 98 parts of the total anionic surfactant by weight present in the spray-dried particle.
- alkali metal silicate to the partly neutralized anionic surfactant in the aqueous mixture, the remaining unreacted acid form of the anionic surfactant reacts with the alkali metal silicate salt to form fully neutralized salt form of the anionic surfactant.
- a fully neutralized anionic surfactant is added to the aqueous mixture.
- liquid acid anionic surfactant precursor is reacted with an alkali metal hydroxide to form fully neutralized anionic surfactant salt before addition to the aqueous mixture. More preferably the liquid acid precursor of the anionic surfactant is partly or fully neutralized in-situ.
- the detersive surfactant is present when the alkaline earth metal salt is contacted with the alkali metal silicate salt.
- the order of addition is to contact the pre-neutralized detersive surfactant or the acid detersive surfactant precursor with water followed by contacting with the alkali metal silicate and then adding the alkaline earth metal salt.
- the part or full neutralization may be carried out in the same vessel by contacting the acid form of the anionic surfactant with an aqueous solution of neutralizing agent (alkali metal hydroxide) to form the neutralized anionic surfactant salt.
- the order of addition may be reversed wherein the step involves adding alkaline earth metal salt to the aqueous mixture followed by the alkali metal silicate salt.
- Suitable detersive surfactants include anionic detersive surfactants, non-ionic detersive surfactant, cationic detersive surfactants, zwitterionic detersive surfactants and amphoteric detersive surfactants.
- Suitable detersive surfactants may be linear or branched, substituted or un-substituted, and may be derived from sources well known to the person skilled in the art.
- the detersive surfactant is an anionic surfactant.
- Suitable anionic detersive surfactants include sulphonate and sulphate surfactants.
- Suitable sulphonate surfactants include methyl ester sulphonate, alpha olefin sulphonate, alkyl benzene sulphonate, especially alkyl benzene sulphonate, preferably Cio to C1 3 alkyl benzene sulphonate.
- a preferred detersive anionic surfactant is linear alkyl benzene sulphonate, where the alkyl chain has 5 to 20 carbon atoms, more preferably the linear alkylbenzene sulphonate surfactant has a C12 to C1 8 alkyl group.
- Suitable alkyl benzene sulphonate (LAS) is obtainable, preferably obtained, by sulphonating commercially available linear alkyl benzene (LAB); suitable LAB includes low 2-phenyl LAB, other suitable LAB includes high 2-phenyl LAB, such as those supplied by Sasol under the tradename Hyblene®.
- Suitable sulphate surfactants include alkyl sulphate, preferably Cs to Ci 8 alkyl sulphate, or predominantly C12 to Cis alkyl sulphate.
- One or more anionic surfactant may be present in the spray-dried detergent particle.
- a preferred sulphate detersive surfactant is alkyl alkoxylated sulphate, preferably alkyl ethoxylated sulphate, preferably a Cs to Cis alkyl alkoxylated sulphate, preferably a Cs to Cis alkyl ethoxylated sulphate, preferably the alkyl alkoxylated sulphate has an average degree of alkoxylation of from 0.5 to 20, preferably from 0.5 to 10, preferably the alkyl alkoxylated sulphate is a Cs to Cis alkyl ethoxylated sulphate having an average degree of ethoxylation of from 0.5 to 10, preferably from 0.5 to 5, more preferably from 0.5 to 3 and most preferably from 0.5 to 1.5.
- alkyl sulphate, alkyl alkoxylated sulphate and alkyl benzene sulphonate may be linear or branched, substituted or un-substituted and may be derived from petrochemical material or biomaterial.
- suitable anionic detersive surfactants include, Soaps, alkyl ether carboxylates.
- Suitable anionic detersive surfactants may be in salt form, suitable counter-ions include sodium, calcium, magnesium, amino alcohols, and any combinations thereof. A preferred counterion is sodium.
- the detersive surfactant is anionic surfactant selected from alkyl benzene sulphonate, primary alkyl sulphate, secondary alkyl sulphate, alkyl ether sulphate or mixtures thereof, still preferably selected from linear alkyl benzene sulphonate, alkyl ether sulphate or mixtures thereof, still preferably selected from LAS, SLES or mixtures thereof.
- Suitable non-ionic detersive surfactants are selected from the group consisting of: Cs to C18 alkyl ethoxylates, such as, NEODOL® non-ionic surfactants from Shell; C 6 to C12 alkyl phenol alkoxylates wherein preferably the alkoxylate units are ethyleneoxy units, propyleneoxy units or a mixture thereof; C12 to Cis alcohol and C 6 to C12 alkyl phenol condensates with ethylene oxide/propylene oxide block polymers such as Pluronic® from BASF; alkyl polysaccharides, preferably alkyl polyglycosides; methyl ester ethoxylates; polyhydroxy fatty acid amides; ether capped poly(oxyalkylated) alcohol surfactants and mixtures thereof.
- Cs to C18 alkyl ethoxylates such as, NEODOL® non-ionic surfactants from Shell
- C 6 to C12 alkyl phenol alkoxylates wherein
- Suitable non-ionic detersive surfactants are alkyl polyglucoside and/or an alkyl alkoxylated alcohol.
- Suitable non-ionic detersive surfactants include alkyl alkoxylated alcohols, preferably Cs to Cis alkyl alkoxylated alcohol, preferably a Cs to Cis alkyl ethoxylated alcohol, preferably the alkyl alkoxylated alcohol has an average degree of alkoxylation of from 1 to 50, preferably from 1 to 30, or from 1 to 20, or from 1 to 10, preferably the alkyl alkoxylated alcohol is a Cs to Cis alkyl ethoxylated alcohol having an average degree of ethoxylation of from 1 to 10, preferably from 1 to 7, more preferably from 1 to 5 and most preferably from 3 to 7.
- the alkyl alkoxylated alcohol can be linear or branched and substituted or un-substituted.
- Suitable nonionic detersive surfactants include secondary alcohol-based detersive surfactants.
- Zwitterionic surfactant Suitable zwitterionic detersive surfactants include amine oxides and/or betaines.
- One or more detersive surfactant may be present in the spray-dried particle according to the present invention.
- the surfactants are preferably those which are thermally stable during processing conditions of a tower with inlet air temperature ranging from 250°C to 500°C and those which are chemically stable at the pH conditions of the spray-drying slurry.
- Non-limiting examples of the anionic surfactant includes the ones mentioned above. Step (ii): Forming in-situ silicate salt or disilicate salt of alkaline earth metal
- the alkali metal silicate reacts with the alkaline earth metal salt to form in-situ silicate or disilicate salt of alkaline earth metal or mixtures thereof.
- the alkaline earth metal salt present in the reaction is magnesium sulphate or magnesium chloride, more preferably magnesium sulphate.
- the magnesium sulphate reacts with alkali metal silicate to form in-situ magnesium silicate or magnesium disilicate or mixtures thereof.
- the alkali metal silicate is sodium silicate.
- the reaction of the alkali metal silicate with the alkaline earth metal salt is carried out by heating the aqueous mixture in a mixer at a temperature of 20°C to 80°C, more preferably from 70°C to 80°C.
- the reaction is carried out for a duration of
- the reaction may also produce hydroxide of alkaline earth metal and some amount of the alkaline earth metal salt may remain unreacted. Such that the aqueous mixture may include an amount of unreacted magnesium sulphate.
- the aqueous mixture includes the in-situ formed silicate salt or disilicate salt of alkaline earth metal or mixtures thereof, alkali metal silicate salt, detersive surfactant, any unreacted alkaline earth metal salt and water.
- the resulting aqueous mixture preferably includes:
- the silicate salt or disilicate salt of the alkaline earth metal is 50% amorphous, more preferably 60% amorphous, still preferably 80%, further preferably 90% amorphous. In a highly preferred embodiment, all of the in-situ formed silicate salt and/or disilicate salt of alkaline earth metal salt is amorphous.
- the detersive surfactant is an anionic surfactant.
- the aqueous mixture may include hydroxide of alkaline earth metal and some amount of unreacted alkaline earth metal salt.
- the aqueous mixture after forming the in-situ silicate salt of alkaline earth metal comprises: (i) 0.1 wt.% to 4.5 wt.% in-situ formed silicate salt and/or disilicate salt or of alkaline earth metal.
- the next step involves adding sodium carbonate to form an aqueous slurry.
- 10 wt.% to 62 wt.% of sodium carbonate and a filler selected from the group consisting of alkali metal chloride, alkaline earth metal carbonate or mixtures thereof is added to the aqueous mixture obtained in step (ii) followed preferably by addition of minor laundry ingredients, to form an aqueous slurry.
- the slurry may also include potassium carbonate.
- sodium carbonate makes up at least 75 wt.%, more preferably at least 85 wt.% and even more preferably at least 90 wt.% of the total weight of the carbonate salt.
- inorganic builders include, crystalline and amorphous aluminosilicates for example, zeolites as disclosed in GB 1 473201 (Henkel), amorphous aluminosilicates as disclosed in GB 1 473202 (Henkel) and mixed crystalline/amorphous aluminosilicates as disclosed in GB 1 470 250 (Procter & Gamble); sodium alkaline silicates and layered silicates as disclosed in EP 164514 B (Hoechst).
- the sodium carbonate may be from synthetically prepared or from a natural source. Synthetically prepared soda ash is available commercially as synthetic light soda ash.
- Inorganic phosphate builders for example sodium orthophosphate, pyrophosphate and tripolyphosphate are present at 0 wt.% level.
- the spray-dried detergent particle prepared from the process according to the first aspect of the present invention is substantially free of inorganic phosphate builders. By substantially free it is meant that the spray dried particle prepared according to the process of the first aspect does not include any deliberately added inorganic phosphate builder.
- the aqueous slurry includes 0 wt.% inorganic phosphate builders.
- Zeolite builders used in most commercial particulate detergent compositions is zeolite A.
- aluminium zeolite P zeolite MAP
- zeolite MAP is an alkali metal aluminosilicate of the P type having a silicon to aluminium ratio not exceeding 1.33, preferably not exceeding 1.15, and more preferably not exceeding 1.07.
- Zeolite builders are preferably present at relatively low levels, for example less than 5 wt.%, still preferably less than 3 wt.%, further preferably less than 1 wt.% in the aqueous slurry.
- the spray- dried detergent particle prepared from the process according to the first aspect of the present invention is substantially free of zeolite builders.
- substantially free it is meant that the spray dried particle prepared according to the process of the first aspect does not include any deliberately added inorganic zeolite builder.
- the aqueous slurry includes 0 wt.% zeolite builders.
- the aqueous slurry may include an organic builder.
- organic builder include polycarboxylate polymers such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphinates; monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di-and trisuccinates, carboxy methyl oxysuccinates, carboxymethyloxymalonates, dipicolinates, hydroxyethyliminodiacetates, alkyl- and alkenylmalonates and succinates; and sulphonated fatty acid salts.
- polycarboxylate polymers such as polyacrylates, acrylic/maleic copolymers, and acrylic phosphinates
- monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di-and trisuccinates, carboxy methyl oxysuccinates, carboxymethyloxymalon
- the organic builder is selected from monomeric polycarboxylates such as citrates, gluconates, oxydisuccinates, glycerol mono-, di-and trisuccinates, carboxymethyloxysuccinates, carboxymethyloxymalonates, dipicolinates, hydroxyethyliminodiacetates, alkyl- and alkenylmalonates and succinates, more preferably alkali metal citrate, most preferably it is sodium citrate.
- Organic builders may be used in minor amounts as supplement to carbonate builder.
- Preferred supplementary organic builders are citrates, suitably used in amounts of from 0.1 wt.% to 30 wt.% more preferably of alkaline metal compounds, preferably from 10 wt.% to 25 wt.%; and acrylic polymers, more especially acrylic/maleic copolymers, suitably used in amounts of from 0.5 wt.% to 15 wt.%, preferably from 1 wt.% to 10 wt.%.
- Powder flow properties may be improved by the incorporation of a small amount of a powder structurant, for example, a fatty acid (or fatty acid soap), a sugar, an acrylate or acrylate/maleate polymer.
- a powder structurant for example, a fatty acid (or fatty acid soap), a sugar, an acrylate or acrylate/maleate polymer.
- a powder structurant is fatty acid soap, suitably present in an amount of from 1 wt.% to 5 wt.%.
- aqueous slurry includes but are not limited to, any one or more of the following: soap, sequestrants, calcium chloride, other inorganic salts, fluorescers, foam controllers, foam boosters, dyes, anti redeposition agents, colourants, shading dyes and combinations thereof.
- a filler selected from the group consisting of alkali metal chloride, alkaline earth metal carbonate or mixtures thereof is added to the aqueous slurry before spray-drying.
- the filler may be added either before the addition of the sodium carbonate or after the addition of the sodium carbonate to the aqueous mixture to form the aqueous slurry. It is preferred to add the filler after the addition of the sodium carbonate.
- the filler acts as a balancing ingredient and is preferably selected from the group consisting of sodium chloride, calcium carbonate, magnesium carbonate, calcite, dolomite or mixtures thereof.
- the filler is alkali metal carbonate, more preferably sodium chloride.
- Alkaline earth metal carbonate preferably includes calcium carbonate (calcite), magnesium carbonate, magnesium calcium carbonate (dolomite) or mixtures thereof.
- the amount of alkali metal silicate remaining in the aqueous slurry after forming the in-situ silicate, disilicate of alkaline earth metal is from 3 wt.% to 14 wt.% of the aqueous slurry.
- the aqueous slurry prepared according to the process of the first aspect of the present invention preferably comprises: (i) 5 wt.% to 30 wt.% detersive surfactant, preferably 5 wt.% to 27 wt.% detersive surfactant;
- filler selected from alkali metal chloride, alkaline earth metal carbonate or mixtures thereof, preferably a filler selected from sodium chloride, calcium carbonate, magnesium carbonate, calcite, dolomite, or mixtures thereof;
- (x) optionally organic builder, preferably 0 wt.% to 10 wt.% citrate salt;
- optical brighteners which is preferably selected from fluorescers, colourants, shading dye, pigments or mixtures thereof;
- (xii) optionally antifoams, preferably selected from silicone oil.
- the detersive surfactant present in the aqueous slurry is an anionic surfactant. It may also be a mixture of anionic surfactant and nonionic surfactant where the mixture has a higher content of anionic surfactant.
- the polymer is selected from a cleaning polymer, soil releasing polymer, care polymer, antiredeposition polymer or mixtures thereof.
- the aqueous slurry is spray dried to form a spray-dried particle.
- the spray-drying is carried out using any of the conventional spray drying system known in the art.
- the aqueous slurry is transferred through a pipe system to a pump system consisting of one or more pump and then further to a spray nozzle through which the slurry is released under pressure into a drying tower.
- a typical spray-drying process involves the step of transferring the aqueous slurry through a pipe system leading to a first pump and then through a second pump and from a second pump to a plurality of spray nozzles.
- the first pump is typically a low- pressure pump, such as a pump that can generate a pressure of from 1x10 5 Nnr 2 to 1x10 6 Nnr 2 , which ensures proper flooding of the second pump.
- the second pump is a high-pressure pump, such as a pump that is capable of generating a pressure ranging from 2x10 6 Nnr 2 to 2x10 7 Nnr 2 .
- the aqueous detergent slurry may be transferred through bolt catchers, magnetic filters, lump breakers, disintegrators such as the Ritz Mill, during the transfer of the aqueous slurry through the pipe system downstream the pump system/mixer in which the aqueous slurry is formed.
- the disintegrator is preferably positioned between the pumps.
- the flow rate of the aqueous slurry along the pipes is typically in the range from 800 Kg/hour to more than 75,000 Kg/hour.
- the spray drying system may include a deaeration system.
- the deaeration system is preferably a vacuum assisted de-aerator, which is preferably fed by a transfer pump.
- the deaeration system remove air bubbles formed during the slurry preparation, thus increasing the bulk density of the spray-dried detergent particle.
- De aeration of the slurry may also be carried out by other mechanical means or chemical de-aeration means using antifoams or de-foamers.
- air injection system may be provided along the pipe system.
- the air injection system may be provided before or after the pump system.
- the air injection includes airflow and pressure controls, static mixer, pulsation dampener and compressor set which can aerate the slurry to get a lower bulk density for the spray dried particle.
- the gas injected into the slurry may be nitrogen, carbon dioxide, or simply atmospheric air introduced under a pressure higher than the pressure of the aqueous slurry maintained in the pipe system.
- a typical spray drying system can optionally include both the de-aeration system and air injection system to optimize the desired bulk density of the spray dried particle.
- Typical spray drying tower for detergent applications are counter-current spray drying tower.
- the inlet hot air/hot steam temperature introduced into the spray drying tower is the range from 250°C to 500°C depending on the evaporation capacity and sizing of the tower.
- the tower exhaust air temperature can range from, 60°C to 200°C, more preferably 80°C to 200°C, still more preferably 80°C to 100°C depending on the loading of the tower.
- the aqueous detergent slurry introduced into the spray nozzle of the spray drying tower is preferably at a temperature ranging from 60°C to 95°C.
- the spray drying tower may be a co-current spray drying tower but are less common.
- the spray- dried detergent particle existing the tower is maintained at a temperature less than 150°C, still preferably less than 100°C.
- the spray-drying is preferably conducted where the spray drying zone is under a negative pressure of at least 50 Nrrr 2 , still preferably the negative pressure is from 50 Nrrr 2 to 600 Nnr 2 .
- the vacuum conditions are achieved by controlling the speed and/or dampener setting of the inlet and the outlet air fans.
- the spray-dried particle collected at the bottom of the tower may be subjected to cooling and conditioning by using an air lift or any similar process.
- the spray-dried particle collected from the bottom of the spray-drying tower is preferably mixed with a flow aid chosen from zeolite or similar fine mineral particles selected from dolomite, calcite or mixtures thereof, just before being air-lifted.
- the spray-dried detergent is subject to particle size classification to remove oversize material (> 2 mm typically) to provide a spray dried detergent particle which is free flowing.
- the fine material ⁇ 100 microns typically
- Spray-dried detergent particle
- Spray-dried particle formed from the process of the first aspect of the present invention preferably has a pH of 11.5 or less, preferably a pH ranging from 10.5 to 11.5 when measured using a 1 wt.% solution with distilled water at 25°C.
- the spray-dried particle is generally referred to as the base powder. This base powder may be used as a fully formulated laundry detergent composition.
- the spray-dried detergent particle includes:
- detersive surfactant preferably anionic detersive surfactant
- (x) optionally, from 0 wt.% to 2.5 wt.% unreacted alkaline earth metal salt. It is preferred to keep the moisture content of the spray-dried detergent particle not more than 4.5 wt.% to ensure that the spray-dried particle is free-flowing. Preferably the amount of filler present is 1 wt.% to 67 wt.%.
- the spray-dried detergent particle may include 0 wt.% added sodium sulphate, the spray dried detergent particle may however include in-situ formed sodium sulphate in an amount which is less than 4 wt.%, still preferably less than 1.5 wt.%
- the spray dried detergent particle may preferably include from 0 wt.% to 4 wt.% polymer selected from antiredeposition polymer, soil release polymer, structuring polymer or mixtures thereof.
- the polymer is a polymeric carboxylate, preferably polyacrylate or a copolymer of acrylic acid and maleic acid.
- other polymers may also be suitable such as polyamines (including the ethoxylated variants thereof), polyethylene glycol and polyesters.
- Polymeric soil suspending aids and polymeric soil release agents are particularly suitable.
- the spray-dried detergent particle has a bulk density of less than 550g/L.
- the spray-dried detergent particle has a weight average particle size of from 300 micrometres to 600 micrometres.
- the spray-dried detergent particle comprises from 7 wt.% to 40 wt.% anionic surfactants, which is preferably a Cio to C2 0 linear alkyl benzene sulphonate and which is substantially neutralized with little or no acid residues.
- the spray-dried particle is typically post dosed with ingredients that are incompatible with the spray-drying process conditions to form a fully formulated laundry detergent composition. These components may be incompatible for many reasons including heat sensitivity, pH sensitivity or degradation in aqueous systems.
- Detergent compositions of low to moderate bulk density may be prepared by spray drying the aqueous slurry to form a spray-dried particle and optionally postdosing (dry mixing) further ingredients.
- “compact" detergent compositions may be prepared by further mixing the spray dried particle prepared according to the present invention in a high-speed mixer/granulator, or other non-tower processes.
- the spray dried detergent particle may also be used for preparing a tablet composition by compacting powders, especially "concentrated" powders using the known tableting process.
- the spray dried detergent particle may be used for preparing an unit dose product where the spray-dried detergent particle is enclosed in a pouch, preferably a water-soluble pouch, more preferably a water-soluble pouch comprising a film forming polymer selected from polyvinyl alcohol, polyvinylpyrrolidone and other known film forming polymer.
- the base powder/spray-dried particle is preferably formulated into a finished detergent composition by dry mixing heat sensitive ingredients into the base powder. In addition to heat sensitive ingredients some amount of alkalinity may be added back into the base powder by addition of alkaline ingredients, additionally other acidic or neutral may also be added to formulate the finished detergent composition.
- the spray-dried detergent particle may be used as a fully formulated laundry detergent composition or may be additionally combined with other optional ingredients to form a fully formulated laundry detergent composition.
- the optional post-dosed benefit ingredients includes but is not limited to enzymes, anti-redeposition polymers, perfumes, additional surfactant selected from amphoteric surfactant, zwitterionic surfactant, cationic surfactant and non-ionic surfactant, optical brighteners, antifoaming agent, foam boosters, fabric softeners such as smectite clays, amine softeners and cationic softeners; bleach and bleach activators; dyes or pigments, fillers, fluorescers, salts, soil release polymers, dye transfer inhibitors.
- Non-limiting examples of the post-dosed polymers include cleaning polymers, antiredeposition polymers, soil release polymers structuring polymers.
- Some examples include PET-PEOT polymer (Repel-o-Tex® SF2 ex.Solvay), copolymer of acrylic acid and maleic acid (Sokalan CP5 ex. BASF). Fluorescers
- Suitable fluorescent brighteners include dis-styryl biphenyl compounds example Tinopal® CBS-X, di-amino stilbene di-sulfonic acid compounds, e.g. Tinopal® DMS pure Xtra and Blankophor® HRH, and Pyrazoline compounds, e.g. Blankophor® SN, and coumarin compounds, e.g. Tinopal® SWN.
- Preferred brighteners are: sodium 2 (4- styry)-3-sulfophenyl)-2H-napthol(1,2-d]triazole, disodium 4,4’bis ⁇ [4-anilino-6-(N methyl- N-2 hydroxyethyl)amino 1,3,5- triazin-2-yl)]amino]stilbene-2-2' disulfonate, disodium 4,4’bis([(4-anilino-6-morpholino-l,3,5-triazin-2-yl)]amino ⁇ stilbene-2-2'disulfonate, and disodium 4,4’- bis(2-sulfostyryl)biphenyl.
- a suitable fluorescent brightener is S C.l. Fluorescent Brightener 260, which may be used in its beta or alpha crystalline forms, or a mixture of these forms.
- the composition of the present invention preferably includes an enzyme. It may preferably include one or more enzymes. Preferred examples of the enzymes include those which provide cleaning performance and/or fabric care benefits.
- suitable enzymes include, but are not limited to, hemicellulases, peroxidases, proteases, cellulases, xylanases, lipases, xyloglucanase, phospholipases, esterases, cutinases, pectinases, mannanases, pectate lyases, keratinases, reductases, oxidases, phenoloxidases, lipoxygenases, ligninases, pullulanases, tannases, pentosanases, malanases, G-glucanases, arabinosidases, hyaluronidase, chondroitinase, laccase, and amylases, or mixtures thereof.
- a typical combination is an enzyme cocktail that may comprise, for example, a protease and lipase in conjunction with one or more of amylase, mannanase and cellulase.
- the enzymes When present in a detergent composition, the enzymes may be present at levels from about 0.00001% to about 2%, from about 0.0001% to about 1% or from 0.001% to about 0.5% enzyme protein by weight of the detergent composition.
- the spray dried detergent particle or a laundry composition having the spray dried detergent particle prepared according to the invention may be packaged as unit doses in polymeric film soluble in the wash water.
- the spray-dried detergent particle or a composition including the particle of the invention may be supplied in multidose plastics packs with a top or bottom closure.
- a dosing measure may be supplied with the pack either as a part of the cap or as an integrated system.
- the packaging material suitable for packaging may include but not limited to multilayer polyethylene film, laminate, paper based, and other materials known to a person skilled in the art.
- the packaging material is selected from material which are biodegradable or recyclable.
- a method of laundering fabric using a spray dried detergent particle or a laundry composition comprising a spray dried detergent particle according to the present invention which involves the step of diluting the dose of detergent composition with water to obtain a wash liquor and washing fabrics with the wash liquor so formed.
- the dose of detergent composition is typically put into a dispenser and from there it is flushed into the machine by the water flowing into the machine, thereby forming the wash liquor. From 5 up to about 65 litres of water may be used to form the wash liquor depending on the machine configuration.
- the dose of detergent composition may be adjusted accordingly to give appropriate wash liquor concentrations.
- the dilution step preferably provides a wash liquor which comprises inter alia from about 3 to about 20 g/wash of detersive surfactants (as are further defined above). Examples
- Example 1 Preparing an aqueous slurry and a spray dried detergent particle according to the present invention
- a spray-dried laundry detergent particle according to the present invention was prepared by first mixing water, neutralizing agent (NaOH, 50% aqueous solution) and linear alkyl benzene sulphonic acid in a crutcher where they were agitated to neutralize the linear alkyl benzene sulphonic acid to its salt form. Thereafter an excess of sodium silicate (47% aqueous solution, alkali metal silicate) was added to the aqueous mixture. The sodium silicate has a Na 2 0 to S1O2 ratio of 1:2.4. The addition of sodium silicate was followed by addition of magnesium sulphate (alkaline earth metal salt).
- the aqueous mixture was continuously agitated, and the mixture was heated to a temperature of around 78°C to 80°C upon addition of sodium silicate and the temperature was maintained till the end of the batch preparation.
- the sodium silicate and magnesium sulphate react to form in-situ magnesium silicate or magnesium disilicate or combination of bothr Further sodium carbonate and sodium chloride as filler, was added in this order to form an aqueous slurry.
- the composition of the ingredients added to the form a batch of 10000 Kg aqueous slurry is provided in Table 1.
- Example 1 The aqueous slurry of Example 1 was spray dried to prepare a spray dried detergent particle which was thereafter evaluated.
- the aqueous slurry was spray-dried in a conventional counter current spray drying tower to form a spray dried detergent particle with a moisture content of around 2 wt.% to 3.5 wt.%.
- the composition of the spray dried powder is provided in Table 2 below. Table 2
- the spray-dried detergent particle prepared according to the present invention was evaluated for powder properties as described below. Compression test This test evaluates the tendency of the powder towards caking. A split cylinder with a polished internal surface is positioned on a firm base to form a hollow cylindrical mould with a diameter of 9 centimetres. Spray dried detergent particle prepared according to the present invention (Ex 1) was filled inside the hollow cylindrical mould and levelled. A plastic disc is placed on levelled spray-dried detergent particle mass. A weight of 12 kilogram is slowly placed on the plastic disc in such a way that the weight is uniformly applied on the spray-dried detergent particle mass in the mould and the disc was allowed to compact the spray-dried detergent particle mass to form a compacted cake.
- DFR Dynamic flow rate measurement: The apparatus used for measuring DFR consists of a cylindrical glass tube having an internal diameter of 35 mm and a length of 600 mm. The tube was securely clamped in a position such that its longitudinal axis is vertical. Its lower end was terminated by means of a smooth cone of polyvinyl chloride having an internal angle of 15 and a lower outlet orifice of diameter 225 mm. A first beam sensor is positioned 150 mm above the outlet, and a second beam sensor is positioned 250 mm above the first sensor.
- the outlet orifice was temporarily closed, for example, by covering with a piece of card, and powder is poured through a funnel into the top of the cylinder until the powder level is about 10 cm higher than the upper sensor; a spacer between the funnel and the tube ensures that filling is uniform.
- the averaging and calculation are carried out electronically and a direct read-out of the DFR value obtained.
- a DFR value of higher than 80 mL/s is considered to have good flow properties.
- Example 2 Preparing an aqueous slurry and a spray dried detergent particle according to the present invention
- a spray-dried laundry detergent particle according to the present invention was prepared by first mixing water, neutralizing agent (NaOH, 48% aqueous solution) and linear alkyl benzene sulphonic acid in a crutcher where they were agitated to neutralize the linear alkyl benzene sulphonic acid to its salt form. Thereafter an excess of sodium silicate (42% aqueous solution, alkali metal silicate) was added to the aqueous mixture.
- the sodium silicate has a Na 2 0 to S1O2 ratio of 1:2.4.
- the addition of sodium silicate was followed by addition of magnesium sulphate (alkaline earth metal salt).
- the aqueous mixture was continuously agitated, and the mixture was heated to a temperature of around 78°C to 80°C upon addition of sodium silicate and the temperature was maintained till the end of the batch preparation.
- the sodium silicate and magnesium sulphate react to form in-situ magnesium silicate or magnesium disilicate or combination of bothr Further sodium carbonate and sodium chloride as filler, was added in this order to form an aqueous slurry.
- the ingredients added to the form a batch of 4800 Kg aqueous slurry is provided in Table 3. A. Preparing an aqueous slurry
- the aqueous slurry of Exp 2 was spray dried to prepare a spray dried detergent particle which was thereafter evaluated.
- the aqueous slurry was spray-dried in a conventional counter current spray drying tower to form a spray dried detergent particle with a moisture content of around 2 wt.% to 3.5 wt.%.
- the composition of the spray dried powder is provided in Table 4 below. Table 4
- the data on table 4 shows that the inventive spray dried detergent particle (Ex 2) showed similar powder properties as that of the Control.
- the inventive spray-dried particle was free-flowing as shown by the DFR values (above 80 mL/s) and showed anticaking properties over extended storage life as show by the compression test values (less than 1Kg).
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)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP21174575 | 2021-05-19 | ||
PCT/EP2022/063252 WO2022243276A1 (en) | 2021-05-19 | 2022-05-17 | Process for preparing a spray dried detergent particle |
Publications (1)
Publication Number | Publication Date |
---|---|
EP4341368A1 true EP4341368A1 (en) | 2024-03-27 |
Family
ID=76011743
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP22729211.7A Pending EP4341368A1 (en) | 2021-05-19 | 2022-05-17 | Process for preparing a spray dried detergent particle |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP4341368A1 (en) |
CN (1) | CN117255848A (en) |
BR (1) | BR112023024016A2 (en) |
WO (1) | WO2022243276A1 (en) |
Family Cites Families (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5335081B1 (en) | 1971-06-30 | 1978-09-25 | ||
AT330930B (en) | 1973-04-13 | 1976-07-26 | Henkel & Cie Gmbh | PROCESS FOR THE PRODUCTION OF SOLID, SPILLABLE DETERGENTS OR CLEANING AGENTS WITH A CONTENT OF CALCIUM BINDING SUBSTANCES |
DE2433485A1 (en) | 1973-07-16 | 1975-02-06 | Procter & Gamble | ALUMINOSILICATE ION EXCHANGERS SUITABLE FOR USE IN DETERGENTS |
DE2413561A1 (en) | 1974-03-21 | 1975-10-02 | Henkel & Cie Gmbh | STORAGE-RESISTANT, EASILY-RELEASE DETERGENT ADDITIVE AND METHOD FOR MANUFACTURING IT |
US4139486A (en) | 1977-03-22 | 1979-02-13 | The Procter & Gamble Company | Built detergent composition |
DE3413571A1 (en) | 1984-04-11 | 1985-10-24 | Hoechst Ag, 6230 Frankfurt | USE OF CRYSTALLINE LAYERED SODIUM SILICATES FOR WATER SOFTENING AND METHOD FOR WATER SOFTENING |
CA2001927C (en) | 1988-11-03 | 1999-12-21 | Graham Thomas Brown | Aluminosilicates and detergent compositions |
WO2005037712A1 (en) | 2003-10-20 | 2005-04-28 | Theo Jan Osinga | Method for the preparation of a suspension |
GB0420356D0 (en) | 2004-09-13 | 2004-10-13 | Unilever Plc | Detergent compositions and their manufacture |
ES2442541T3 (en) | 2008-06-25 | 2014-02-12 | The Procter & Gamble Company | Process to prepare a detergent powder |
EP2138565A1 (en) | 2008-06-25 | 2009-12-30 | The Procter and Gamble Company | A spray-drying process |
-
2022
- 2022-05-17 CN CN202280032434.2A patent/CN117255848A/en active Pending
- 2022-05-17 BR BR112023024016A patent/BR112023024016A2/en unknown
- 2022-05-17 WO PCT/EP2022/063252 patent/WO2022243276A1/en active Application Filing
- 2022-05-17 EP EP22729211.7A patent/EP4341368A1/en active Pending
Also Published As
Publication number | Publication date |
---|---|
BR112023024016A2 (en) | 2024-02-06 |
CN117255848A (en) | 2023-12-19 |
WO2022243276A1 (en) | 2022-11-24 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US7387992B2 (en) | Laundry detergent with polyamine mono-anionic surfactant | |
US20060035802A1 (en) | Highly water-soluble solid laundry detergent composition that forms a clear wash liquor upon dissolution in water | |
US4552681A (en) | Granular, free-flowing detergent component and method for its production | |
US20090286711A1 (en) | Solid Laundry Detergent Composition Comprising Light Density Silicate Salt | |
EP2841553B1 (en) | Process for the production of a detergent granule, detergent granule and detergent composition comprising said granule | |
EP3030641B1 (en) | Process for the production of a detergent granule, detergent granule and detergent composition comprising said granule | |
AU768794B2 (en) | Particulate detergent composition containing zeolite | |
EP4341368A1 (en) | Process for preparing a spray dried detergent particle | |
EP2870229A1 (en) | Process for the production of a detergent granule, detergent granule and detergent composition comprising said granule | |
EP4341367A1 (en) | Process for preparing a spray dried detergent particle | |
WO2022243283A1 (en) | Process for preparing a spray dried detergent particle | |
EP4341366A1 (en) | Process for preparing a spray dried detergent particle | |
US5998356A (en) | Process for making granular detergents | |
EP4402232A1 (en) | Process for preparing a spray dried detergent particle | |
WO2022243343A1 (en) | Process for preparing a spray dried detergent particle | |
EP4402234A1 (en) | Process for preparing a spray dried detergent particle | |
EP4402231A1 (en) | Process for preparing a spray dried detergent particle | |
EP4402233A1 (en) | Process for preparing a spray dried detergent particle | |
EP1185603B1 (en) | Granular detergent composition containing zeolite map | |
WO2024088878A1 (en) | Spray-dried laundry particle | |
WO2023057437A1 (en) | Laundry composition | |
MXPA01012731A (en) | Process for preparing granular detergent compositions. |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: UNKNOWN |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE INTERNATIONAL PUBLICATION HAS BEEN MADE |
|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE |
|
17P | Request for examination filed |
Effective date: 20231018 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: GRANT OF PATENT IS INTENDED |
|
DAV | Request for validation of the european patent (deleted) | ||
DAX | Request for extension of the european patent (deleted) | ||
INTG | Intention to grant announced |
Effective date: 20240715 |