EP2121588A2 - Solid detergent composition and process to prepare the same - Google Patents
Solid detergent composition and process to prepare the sameInfo
- Publication number
- EP2121588A2 EP2121588A2 EP08717440A EP08717440A EP2121588A2 EP 2121588 A2 EP2121588 A2 EP 2121588A2 EP 08717440 A EP08717440 A EP 08717440A EP 08717440 A EP08717440 A EP 08717440A EP 2121588 A2 EP2121588 A2 EP 2121588A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- magnesium
- detergent composition
- solid detergent
- builder
- solid
- 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- Withdrawn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
- 238000000034 method Methods 0.000 title claims abstract description 76
- 239000000203 mixture Substances 0.000 title claims description 80
- 239000013042 solid detergent Substances 0.000 title claims description 34
- 239000002253 acid Substances 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 150000004996 alkyl benzenes Chemical class 0.000 claims abstract description 28
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011777 magnesium Substances 0.000 claims abstract description 25
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 25
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 24
- 239000007787 solid Substances 0.000 claims abstract description 20
- 239000003513 alkali Substances 0.000 claims abstract description 19
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 19
- 239000011541 reaction mixture Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims description 38
- 239000008187 granular material Substances 0.000 claims description 26
- 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 claims description 15
- 238000007580 dry-mixing Methods 0.000 claims description 15
- 239000011734 sodium Substances 0.000 claims description 15
- 229910052708 sodium Inorganic materials 0.000 claims description 15
- 239000011256 inorganic filler Substances 0.000 claims description 9
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 9
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical class OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 8
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 8
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 8
- 239000001095 magnesium carbonate Substances 0.000 claims description 8
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 7
- 239000010457 zeolite Substances 0.000 claims description 7
- UREZNYTWGJKWBI-UHFFFAOYSA-M benzethonium chloride Chemical compound [Cl-].C1=CC(C(C)(C)CC(C)(C)C)=CC=C1OCCOCC[N+](C)(C)CC1=CC=CC=C1 UREZNYTWGJKWBI-UHFFFAOYSA-M 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- 239000010459 dolomite Substances 0.000 claims description 6
- 229910000514 dolomite Inorganic materials 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 235000021317 phosphate Nutrition 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 150000001340 alkali metals Chemical class 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000000454 talc Substances 0.000 claims description 4
- 229910052623 talc Inorganic materials 0.000 claims description 4
- 238000004448 titration Methods 0.000 claims description 4
- 229910021536 Zeolite Inorganic materials 0.000 claims description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 150000004760 silicates Chemical class 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
- 229910000503 Na-aluminosilicate Inorganic materials 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000318 alkali metal phosphate Inorganic materials 0.000 claims description 2
- 239000001506 calcium phosphate Substances 0.000 claims description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 2
- 235000011010 calcium phosphates Nutrition 0.000 claims description 2
- 239000000378 calcium silicate Substances 0.000 claims description 2
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 2
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 2
- 150000001860 citric acid derivatives Chemical class 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 claims description 2
- 239000002370 magnesium bicarbonate Substances 0.000 claims description 2
- 229910000022 magnesium bicarbonate Inorganic materials 0.000 claims description 2
- 235000014824 magnesium bicarbonate Nutrition 0.000 claims description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- 239000004137 magnesium phosphate Substances 0.000 claims description 2
- 229910000157 magnesium phosphate Inorganic materials 0.000 claims description 2
- 229960002261 magnesium phosphate Drugs 0.000 claims description 2
- 235000010994 magnesium phosphates Nutrition 0.000 claims description 2
- 239000000391 magnesium silicate Substances 0.000 claims description 2
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 2
- 235000019792 magnesium silicate Nutrition 0.000 claims description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 2
- 239000000429 sodium aluminium silicate Substances 0.000 claims description 2
- 235000012217 sodium aluminium silicate Nutrition 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 2
- 239000003826 tablet Substances 0.000 claims description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 2
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 2
- OUHCLAKJJGMPSW-UHFFFAOYSA-L magnesium;hydrogen carbonate;hydroxide Chemical compound O.[Mg+2].[O-]C([O-])=O OUHCLAKJJGMPSW-UHFFFAOYSA-L 0.000 claims 1
- 239000003599 detergent Substances 0.000 description 46
- 239000000047 product Substances 0.000 description 30
- 239000004094 surface-active agent Substances 0.000 description 28
- 230000003472 neutralizing effect Effects 0.000 description 17
- -1 alkaline earth metal salt Chemical class 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 16
- 239000003795 chemical substances by application Substances 0.000 description 15
- 238000004140 cleaning Methods 0.000 description 15
- 238000009472 formulation Methods 0.000 description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000004744 fabric Substances 0.000 description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- 230000008901 benefit Effects 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 8
- 125000000217 alkyl group Chemical group 0.000 description 7
- 239000003945 anionic surfactant Substances 0.000 description 7
- 239000004615 ingredient Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000003082 abrasive agent Substances 0.000 description 6
- 125000004432 carbon atom Chemical group C* 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 5
- 150000007513 acids Chemical class 0.000 description 5
- 125000002091 cationic group Chemical group 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 description 5
- 235000017550 sodium carbonate Nutrition 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002736 nonionic surfactant Substances 0.000 description 4
- 235000011837 pasties Nutrition 0.000 description 4
- 239000012265 solid product Substances 0.000 description 4
- 229910021532 Calcite Inorganic materials 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 150000001339 alkali metal compounds Chemical class 0.000 description 2
- 150000001341 alkaline earth metal compounds Chemical class 0.000 description 2
- 125000002947 alkylene group Chemical group 0.000 description 2
- 125000000129 anionic group Chemical group 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- JUSBJERCRFVSOW-UHFFFAOYSA-L magnesium;oxido hydrogen carbonate Chemical compound [Mg+2].OC(=O)O[O-].OC(=O)O[O-] JUSBJERCRFVSOW-UHFFFAOYSA-L 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000012044 organic layer Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- SIDULKZCBGMXJL-UHFFFAOYSA-N 1-dimethylphosphoryldodecane Chemical compound CCCCCCCCCCCCP(C)(C)=O SIDULKZCBGMXJL-UHFFFAOYSA-N 0.000 description 1
- KRUABTDBQQLWLS-UHFFFAOYSA-N 1-methylsulfinyltetradecane Chemical compound CCCCCCCCCCCCCCS(C)=O KRUABTDBQQLWLS-UHFFFAOYSA-N 0.000 description 1
- MRYUEHRAIMRPNB-UHFFFAOYSA-O 5-methyl-6-phenylphenanthridin-5-ium-3,8-diamine Chemical compound C12=CC(N)=CC=C2C2=CC=C(N)C=C2[N+](C)=C1C1=CC=CC=C1 MRYUEHRAIMRPNB-UHFFFAOYSA-O 0.000 description 1
- MQOKYEROIFEEBH-UHFFFAOYSA-N 5-methyl-6-phenylphenanthridin-5-ium-3,8-diamine;bromide Chemical group [Br-].C12=CC(N)=CC=C2C2=CC=C(N)C=C2[N+](C)=C1C1=CC=CC=C1 MQOKYEROIFEEBH-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 241000282320 Panthera leo Species 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- FIMJSWFMQJGVAM-UHFFFAOYSA-N chloroform;hydrate Chemical compound O.ClC(Cl)Cl FIMJSWFMQJGVAM-UHFFFAOYSA-N 0.000 description 1
- 235000015165 citric acid Nutrition 0.000 description 1
- 229940096386 coconut alcohol Drugs 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- SYELZBGXAIXKHU-UHFFFAOYSA-N dodecyldimethylamine N-oxide Chemical compound CCCCCCCCCCCC[N+](C)(C)[O-] SYELZBGXAIXKHU-UHFFFAOYSA-N 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- 150000002681 magnesium compounds Chemical class 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- MPQXHAGKBWFSNV-UHFFFAOYSA-N oxidophosphanium Chemical group [PH3]=O MPQXHAGKBWFSNV-UHFFFAOYSA-N 0.000 description 1
- 235000020030 perry Nutrition 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000002888 zwitterionic surfactant Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
-
- 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
-
- 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
- C11D11/04—Special methods for preparing compositions containing mixtures of detergents by chemical means, e.g. by sulfonating in the presence of other compounding ingredients followed by neutralising
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0047—Detergents in the form of bars or tablets
- C11D17/0065—Solid detergents containing builders
- C11D17/0073—Tablets
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
- C11D17/065—High-density particulate detergent compositions
-
- 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
- C11D3/06—Phosphates, including polyphosphates
-
- 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
Definitions
- the invention relates to a novel and selective process for preparing solid form of magnesium salt of linear alkyl benzene sulphonic acid at high concentration levels and to detergent composition having very high levels of this active surfactant.
- the invention more particularly relates to a non-tower process for preparing solid detergent composition which on the one hand gives all the processing convenience and economic advantages of high-active powder processes and on the other hand gives all the advantageous product attributes presently possible with only the tower drying process e.g high active surfactant levels and concomitant formulation flexibility and relatively low bulk density.
- the invention also relates to a solid detergent composition containing a novel selective combination of surfactants and builders. The compositions and the process to prepare them are suited to the cleaning of fabric or hard surfaces. It is also possible to use the process and product of the invention in personal washing applications like skin and hair cleansing.
- Cleaning compositions either for fabric washing applications or for cleaning hard surfaces generally have soaps or synthetic surfactants as the active ingredients. While soaps have traditionally been used for such purposes, over the last several decades the trend has generally been to use synthetic surfactant based detergent formulations for fabric washing and hard surface cleaning. Synthetic surfactants are made from neutralization of long chain acids available from petroleum processing streams. Advantages of synthetic surfactants are their availability at competitive price and cleaning performance in a wide range of hard water for fabric washing application.
- One such widely used class of synthetic surfactant is the linear alkyl benzene sulphonates (LAS) especially the sodium salt.
- LAS linear alkyl benzene sulphonates
- Sodium LAS based formulations have been traditionally prepared by neutralization of the linear alkyl benzene sulphonic acid with sodium carbonate solution/caustic or any other basic alkali. After neutralization with soda/caustic other formulation ingredients are added to prepare a uniform/ homogeneous slurry. This slurry is then spray dried to give the detergent powder and this process is known as the Tower route.
- An advantage of the tower route is that sodium LAS can be prepared in relatively high levels of active surfactant levels of up to 50%.
- the sodium LAS formulation produced by the tower process also tends to have a low bulk density generally in the range of 0.5 to 0.7 g/cm 3 and a high rate of dissolution in water, both of which are highly preferred by the consumer.
- the disadvantage with the tower route is that spray drying is a relatively expensive process .
- liquid actives e.g. non-ionic surfactants
- US4146551 (Lion, 1979) describes a process for producing the magnesium salt of sulphonic acids and sulfuric esters comprising the step of neutralizing the sulphonic acids and sulphuric esters with an aqueous dispersion containing (1) at least one neutralizing agent selected from the group consisting of magnesium oxide and magnesium hydroxide and (2) at least one neutralizing accelerator selected from the group consisting of benzoic acid, citric acid, malic acid, phosphoric acid, polyphosphoric acid and water soluble salts thereof under a pH of not more than approximately 6.
- This publication teaches aqueous phase reaction of sulphonic acids with magnesium neutralizing agent and so powder/granule forms of the products will have to be prepared using spray drying in the tower route which is not required in the present process.
- EP0135920 (Dresser, 1985) describes a process for making alkaline earth metal salt of alkyl/aryl sulfonic acids where the alkaline earth metal oxide used for neutralization is calcium oxide. The reaction is not carried out in the dry mixing condition but in a slurry state where the reactants are dispersed in organic solvents. The present invention does not require the use of organic solvents. The above publication also does not specifically teach neutralization with magnesium compounds.
- Indian patent application 225/MUM/2000 (Hindustan Lever Ltd, published in 2003) describes a synergistic abrasive cleaning composition containing selective combination of surfactants and a process for producing the same.
- the process comprises neutralization of at least 40% of the acid precursor of the anionic surfactant using at least one mineral of the dolomites group and mixing abrasives and other conventional ingredients such that the total amount of surfactant is between 0.5 and 35% and the amount of abrasives is 30-95% and processing the mixture in a regular manner.
- Dolomite is a mineral having the chemical formula CaMg (003)2 '
- the present inventors have found that using dolomite it is not possible to get higher than 35% active surfactant level which can be processed in the form of powders/granules or extruded into bars while with the process of the present invention it is possible to get surfactant levels as high as 90%. Further this published Indian patent application uses high levels of water outside the selective range of water over which the present invention can be worked for preparation of salt of LAS.
- a process to prepare solid form of magnesium salt of linear alkyl benzene sulphonic acid which comprises the step of neutralization of linear alkyl benzene sulphonic acids with a magnesium based alkali in the presence of 3 to 28% water by weight of the reaction mixture in a high shear mixer .
- the invention is directed to manufacture of solid form of magnesium salt of linear alkyl benzene sulphonic acid.
- solid form is meant the powder or granule form or in the form of an extrudable bar.
- the invention is highly selective in the neutralizing agent which is used for neutralization of the linear alkyl benzene sulphonic acids in that only magnesium based alkalis have been found to give this unique combination of processing convenience and desired product attributes.
- Other alkali and alkaline earth metal compounds have been used in the past but each one of them has certain drawbacks which are overcome by using the selective magnesium based alkalis of the present invention.
- alkali metal compounds of sodium or potassium With the use of alkali metal compounds of sodium or potassium the highest active levels that has been possible to make has been in the range of 35 to 40%.
- the sodium or potassium LAS obtained is at best a pasty mass and high levels of inorganic fillers are needed to get the product in a free flowing powder/granule form or to enable the product to be extruded into bars.
- the present inventors have also tried other alkaline earth metal compounds like those of calcium like calcium hydroxide, carbonate or oxide. It has been determined that amount of the calcium containing neutralizing agent that is needed is far in excess of stoichiometric, generally in the range of 5 to 10 times of stoichiometric requirement in order to get the desired conversion.
- the present inventors have also tried other metals compounds like those of zinc and aluminium but these neutralizing agents produce similar or different processing difficulties.
- magnesium based alkalis for neutralization of the LAS acid excellent conversion could be obtained with as little as 5-100% stoichiometric excess of the magnesium based alkali, more preferably with as little as 5-25% stoichometric excess.
- the process disclosed herein is to prepare a solid form of magnesium salt of linear alkyl benzene sulphonic acid comprising the step of neutralising linear alkyl benzene sulphonic acid with a magnesium based alkali in the presence of 3 to 28% water in a high shear mixer.
- Linear alkylbenzene sulphonic acid is a multi component system of different alkyl chain lengths (R) and position of substitution of the ring in the alkyl chain.
- the chain length distribution generally ranges from C9 to C13 or C14.
- the linear alkyl benzene sulphonic acid is preferably used in the process in amounts in the range of 5 to 90%, more preferably in the range of 10 to 80%, and most preferably 20 to 50% by total weight of reaction mixture.
- the magnesium based alkali may be magnesium carbonate, magnesium bicarbonate, magnesium oxide, magnesium hydroxyl carbonate or magnesium hydroxide, more preferably magnesium carbonate, magnesium hydroxyl carbonate or magnesium oxide.
- the preferred amounts of magnesium based alkali that is added to the reaction mixture is in amounts in the range of 1.5 to 45%, more preferably 2 to 25% by weight of the reaction mixture.
- the reaction is carried out essentially in the dry mixing state i.e the amount of water added is very low.
- the amount of water added is in the range of 3 to 28%, more preferably 4 to 20%, most preferably 4 to 15% by weight of the reaction mixture. A different amount of water needs to be added depending on the amount of LAS acid used and the neutralising agent used.
- Suitable water insoluble inorganic fillers are talc, calcium carbonate, china clay, silica, sodium aluminosilicate, zeolite, calcium phosphate, calcium silicate, dolomite, magnesium phosphate, magnesium silicate or a clay.
- magnesium based alkali as 5 to 100 mol% stoichiometric excess of magnesium based alkali is used for reaction with linear alkyl benzene sulphonic acid.
- the more preferred range is 5 to 25 mole % stoichiometric excess of magnesium based alkali.
- the reaction is carried out in a high shear mixer, preferably with a kneading action.
- the preferred mixers include ploughshare mixer, mixers with kneading members of sigma type, or multi wiping overlap, single curve or double arm.
- the double arm kneading mixers can be of overlapping or tangential in design.
- the high shear kneader mixers are provided with cutters to enable reduction of lump formation. Alternatively the process can be carried out in a helical screw agitator vessel.
- the process requires minimal energy input.
- the reactants can be mixed at room temperature i.e anywhere from 10 to 50 0 C. Suitable reaction time is from 5 to 60 minutes.
- LAS acid is known to be highly corrosive and therefore the neutralization of the LAS acid to the active surfactant is generally carried out in factories located close to the petrochemical producing locations. With the known processes in the prior art, it has not been possible to prepare active surfactant concentrate at higher than 35 to 40% concentration. The general practice has been to form the sodium salt of LAS acid at about 35 to 40% active concentration in factories close to the petrochemical locations. These 35 to 40% surfactant concentrates are then transported to detergent formulation factories which may be geographically distant from the petrochemical factories. Thus there has been a lot of energy and cost spent in transporting the balance 60 to 65% of the surfactant concentrates which may be water or inorganic fillers which adds to the cost to the consumer.
- surfactant concentrates at as high as 85% can be prepared in factories located close to the petrochemicals complexes and then shipped or transported to the detergent formulation factories. This will help in reducing the transportation and therefore the overall cost of the product, in addition to all the advantages already discussed earlier.
- magnesium salt of LAS has attained the desired solid form as a mixture of magnesium salt of LAS acid along with any residual magnesium based alkali and water, other optional ingredients may be added.
- a process for preparation of a solid detergent composition comprising the step of dry mixing a builder with the magnesium salt of linear alkyl benzene sulphonic acid prepared by the first aspect of the invention.
- the amount of magneisum LAS in this process is preferably in an amount in the range of 5 to 90 wt% by weight of the solid detergent composition.
- the process for preparation of the solid detergent composition by dry mixing preferably has 5 to 70 % builder by weight of the solid detergent composition.
- the builder is preferably chosen from alkali metal carbonates, bicarbonates, phosphates, citrates, silicates or zeolites, especially Zeolite A.
- the more preferred builders are alkali metal carbonate, bicarbonate or tripolyphosphate .
- Preferred alkali metal is sodium.
- the process of the invention is capable of producing solid detergent active in very high levels, detergent compositions in the form of bars, powders and granules having very high levels of detergent active can be prepared without the need of conventional water insoluble structurants .
- the process of the invention gives very high flexibility to the detergent formulator in adding a wide variety of liquid/pasty detergent additives and benefit agents. It is also possible to add high levels of liquid non-ionic surfactants.
- the solid detergent composition prepared by the process of the invention can be used to make from as low as 5% to as high as 90 % magnesium salt of linear alkyl benzene sulphonate by weight of the detergent composition.
- a solid detergent composition comprising (i) 5 to 90 % magnesium salt of linear alkyl benzene sulphonic acid; and (ii) 5 to 70 % builder.
- a suitable method to prepare the magnesium salt of linear alkyl benzene sulphonic acid in the detergent composition is by using the process described above.
- the amount of magnesium salt of linear alkyl benzene sulphonic acid can be suitably varied within this range as per the requirement.
- the amount of magnesium LAS may be in the range of 5 to 15%.
- Premium laundry powders may have Magnesium LAS anywhere from 15 to 30% by weight of the detergent composition.
- the magnesium LAS content may be anywhere from 5 to 15% by weight of the composition.
- the solid detergent composition of the present invention comprises builder which is preferably chosen from alkali metal carbonate, bicarbonate, phosphate, citrate, silicate or zeolites. These builders are preferably present from 5 to 60% , most preferably from 10 to 35% by weight of the detergent composition. Highly preferred builders are alkali metal carbonate or phosphate. Most preferred alkali metal is sodium.
- the solid detergent composition comprises a minimum of 2% water. When the process is used to prepare the solid detergent composition not more than 28% water is required to get the product in the desired solid shape and form.
- detergent composition it is possible that higher amounts of water can be added at a later stage and water content of the composition can be as high as 30%.
- the most suitable product forms of the solid detergent composition are the powder, granule, tablet or bar form, most preferred being the powder or granule form.
- the bulk density of the product is generally less than 0.9 g/cm 3 .
- the solid detergent composition has a rate of dissolution that is desired by the consumers.
- the values are in the range of 0.5 to 0.8 g/litre in 10 minutes as measured using the hyamine titration method.
- the method of hyamine titration is given below.
- An aqueous solution of the sample (detergent powder/bar) is titrated with a standard cationic active solution (Hyamine 1622) in a two-phase water-chloroform system using a mixed indicator (Disulfine Blue-Dimidium Bromide) .
- Cationic dye is dimidium bromide and anionic dye is disulfine blue.
- the anionic surfactant forms a salt with the cationic dye (dimidium anionic surfactant salt) which dissolves in the chloroform layer to give the organic layer a pink color.
- the cationic dye diimidium anionic surfactant salt
- the end point is reached when the Hyamine cation displaces the dimidium cation from the chloroform soluble salt and the pink color leaves the chloroform layer as the dye passes to the aqueous phase.
- trace of cationic surfactant disulfine blue salt enters in organic layer where a faint blue tint appears in this layer.
- Hyamine added in excess forms a salt with the anionic dye disulphine blue, which dissolves in the chloroform layer and colors it blue.
- the solid detergent composition is substantially free of organic solvents.
- Liquid/pasty actives include non-ionic surfactants and anionic surfactants like alpha olefin sulphonates (AOS) and primary alkyl sulphates (PAS) .
- AOS alpha olefin sulphonates
- PAS primary alkyl sulphates
- Suitable nonionic detergent surfactant compounds can be broadly described as compounds produced by the condensation of alkylene oxide groups, which are hydrophilic in nature, with an organic hydrophobic compound which may be aliphatic or alkyl aromatic in nature.
- the length of the hydrophilic or polyoxyalkylene radical which is condensed with any particular hydrophobic group can be readily adjusted to yield a water-soluble compound having the desired degree of balance between hydrophilic and hydrophobic elements.
- Particular examples include the condensation product of aliphatic alcohols having from 8 to 22 carbon atoms in either straight or branched chain configuration with ethylene oxide, such as a coconut oil ethylene oxide condensate having from 2 to 15 moles of ethylene oxide per mole of coconut alcohol; condensates of alkylphenols whose alkyl group contains from 6 to 12 carbon atoms with 5 to 25 moles of ethylene oxide per mole of alkylphenol; condensates of the reaction product of ethylenediamine and propylene oxide with ethylene oxide, the condensate containing from 40 to 80% of polyoxyethylene radicals by weight and having a molecular weight of from 5,000 to 11,000; tertiary amine oxides of structure R3NO, where one group R is an alkyl group of 8 to 18 carbon atoms and the others are each methyl, ethyl or hydroxyethyl groups, for instance dimethyldodecylamine oxide; tertiary phosphine oxides of structure R
- the nonionic can also be selected from a range of alkyl poly glucosides. It is possible to have higher levels of nonionic surfactant in the detergent composition as compared to sodium LAS based formulations, without compromising on the desirable product properties like free flow in powders.
- the solid detergent composition may comprise any other anionic surfactant which may be alkali or alkaline earth metal, alkanolamine or ammonium salts of precursor acids, or may comprise cationic amphoteric or zwitterionic surfactants to provide specific functionalities.
- the total amount of such optional synthetic surfactants will generally be up to a maximum of 35% of the composition.
- amphoteric, cationic or zwitterionic detergent surfactants in the compositions .
- detergent-surfactant compounds are compounds commonly used as surface-active agents given in the well-known textbooks "Surface Active Agents", Volume I by Schwartz and Perry and “Surface Active Agents and Detergents", Volume II by Schwartz, Perry and Berch.
- abrasives are generally added to the detergent composition.
- Suitable abrasives are selected from, particulate zeolites, calcites, dolomites, feldspar, silicas, silicates, other carbonates, aluminas, bicarbonates, borates, sulphates and polymeric materials such as polyethylene.
- Preferred abrasives for use in general purpose compositions have a Moh hardness 2-7 although higher hardness abrasives can be employed for specialist applications.
- Preferred average particle sizes for the abrasive fall in the range 0.5-400 microns preferably 10-200 microns.
- Preferred levels of abrasive range from 30 to 85wt% of the composition.
- composition can contain other ingredients that aid in their cleaning performance.
- Composition can also contain, in addition to the ingredients already mentioned, various other optional ingredients such as structurants, colourants, whiteners, optical brighteners, soil suspending agents, detersive enzymes, compatible bleaching agents (particularly hypohalites) , and preservatives.
- a batch of 5 kg of salt of LAS acid was prepared in a Sigma mixer using amount of reactants as shown in Table-1.
- the process involved taking the indicated amount of metal carbonate in the mixer at about 25 0 C.
- LAS acid was added slowly onto the powder with the Sigma mixer blades running to bring it to a homogeneous mixture.
- indicated amount of water was added under mixing to enable neutralization of the LAS acid.
- the total time for neutralization was about 10 minutes.
- the temperature of the neutralized mass was in the range of 40 to 65 0 C.
- the mixer was run for a further ten minutes to get the final product.
- Dolomite is a natural mined material having the structure CaMg(COs) 2 .
- the data in Table-1 for Example - 1 indicates that solid detergent active can be prepared in very high concentrations (>80%) using magnesium based alkali for netralisation of the LAS acid in a high shear mixer.
- the amount of neutralizing agent (magnesium carbonate) required is minimal (only 10% stoichiometric excess) and a highly user friendly product as free flowing powder is achieved.
- the data for Comparative examples A, B and C indicates that not more than 35 wt% detergent active in solid form can be prepared using any of the known neutralizing agents (soda, calcite or dolomite) . Further the amount of neutralizing agent required is several fold that required by stoichiometry to get a solid product, yet the solid product has poor downstream processing properties.
- Table - 2 indicates that a selective amount of water in the range of 3 to 28 weight % is necessary in order to prepare magnesium salt of LAS acid through the dry mixing route .
- Comparative Example - G and Examples 8 to 12 Effect of amount of magnesium carbonate used for neutralization Several experiments were conducted to study the effect of amount of neutralizing agent magnesium carbonate on the product characteristics. The process as described for Example-1 was used for these experiments with the water content added at 8% and the detergent active amounts at 82.2weight %. The results are summarized in Table- 3. Comparative examples A to C are reproduced in this table for comparison with the results obtained as per the examples within the invention (Examples 8 to 12) .
- Comparative Examples H and I and Examples 13 to 17 Many samples of magnesium salt of LAS acid were prepared at various conditions to study the hygroscopic characteristics of the products produced. The samples were prepared using the process as described for Example-1 and the results are summarized in Table-4. The results are compared to two existing commercial samples viz. Surf Excel powder (Comparative Example H) and Wheel Powder (Comparative Example I ) .
- HH condition is at 40 degree C and 96% relative humidity
- Examples 13 to 17 were free flowing powder/ granules after storage at HH condition and comparable to the commercial samples of Surf Excel and Wheel brands.
- the data in Table-4 indicates that the solid detergent active powder/ granule samples prepared as per the invention are not hygroscopic and are acceptable for preparing detergent formulations which can be marketed and get high consumer acceptance .
- Example - 1 Various magnesium LAS based powder and granule detergent compositions were prepared using the process of Example - 1 and the compositional details are shown in Table-5 (Examples 18 to 27) and properties like the bulk density and solubility were measured. The data is compared against properties of commercially available sodium LAS based formulations Surf Excel (Comparative Example J) and Wheel (Comparative Excel K) .
- the filler used was calcite
- the builder used was sodium carbonate
- the electrolyte was sodium sulphate.
- Examples 18 to 27 The data in Table 5 indicates that various compositions as per the invention (Examples 18 to 27) over a wide range of Mg LAS detergent active concentrations and levels of builders and electrolytes gave product of similar or lower bulk density as compared to Na LAS based commercial samples. Further the solubility of the various samples (examples 18 to 27) was high and comparable to the commercial samples of Comparative Examples J and K having sodium LAS.
- Examples 28 to 41 were measured using water at various levels of hardness (0 FH, 48 FH and 72 FH) using various test monitors (WFK 1OD, WFK 2OD, and WFK 30D) which are all test monitors having composite soil on cotton fabric, polycotton and polyester fabric respectively.
- the cleaning performance of comparative examples (28A to 41A) containing conventional sodium LAS based formulations was also measured.
- the hardness was from calcium salts while in the case of 72 FH, 48 FH was from Calcium salt and 24 FH from Magnesium salt.
- the cleaning experiments were as follows :
- the detergent composition was dissolved in a tergo-to-meter pot using 90 rpm speed after which the test monitor was soaked for 15 minutes. The test monitor was then washed in the same tergo-to-meter at 90 rpm for 30 minutes. The test monitor was rinsed three times using an L/C ratio (liquor to cloth ratio) of about 25. The test monitor was then dried, after which the reflectance at 460 nm was measured.
- Table-6 The data on cleaning performance in terms of ⁇ R of the various test monitors of the various examples is summarized in Table - 6.
- concentration of the surfactant, the builder (Sodium carbonate) and electrolyte (Sodium sulphate) are given in gpl (grams per litre of the cleaning solution) .
- Table 6 indicates that the cleaning performance of the detergent compositions of the invention (Examples 28 to 41) is comparable to conventional sodium LAS based formulations of the prior art (Comparative Examples 28A to 41A) when used over a very wide range of water hardness on various types of soil fabrics.
- the invention thus provides for a process to prepare high active detergent solids using a simple and cost effective dry mixing route. With the use of this novel process it is now possible to prepare detergent solids in the powder, granule or extruded bar forms by the dry mixing route which does not require use of high levels of water-insoluble inorganic fillers.
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- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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EP08717440A EP2121588A2 (en) | 2007-03-08 | 2008-03-05 | Solid detergent composition and process to prepare the same |
Applications Claiming Priority (4)
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IN445MU2007 | 2007-03-08 | ||
EP07113313A EP1967512A3 (en) | 2007-03-08 | 2007-07-27 | Solid detergent composition and process to prepare the same |
EP08717440A EP2121588A2 (en) | 2007-03-08 | 2008-03-05 | Solid detergent composition and process to prepare the same |
PCT/EP2008/052692 WO2008107463A2 (en) | 2007-03-08 | 2008-03-05 | Solid detergent composition and process to prepare the same |
Publications (1)
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EP2121588A2 true EP2121588A2 (en) | 2009-11-25 |
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EP07113313A Withdrawn EP1967512A3 (en) | 2007-03-08 | 2007-07-27 | Solid detergent composition and process to prepare the same |
EP08717440A Withdrawn EP2121588A2 (en) | 2007-03-08 | 2008-03-05 | Solid detergent composition and process to prepare the same |
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EP07113313A Withdrawn EP1967512A3 (en) | 2007-03-08 | 2007-07-27 | Solid detergent composition and process to prepare the same |
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EP (2) | EP1967512A3 (en) |
CN (1) | CN101627010A (en) |
BR (1) | BRPI0808550A2 (en) |
WO (1) | WO2008107463A2 (en) |
Families Citing this family (5)
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MX2013001062A (en) * | 2010-07-27 | 2013-02-21 | Unilever Nv | Detergent composition. |
WO2015067438A1 (en) * | 2013-11-07 | 2015-05-14 | Unilever N.V. | Hard surface cleaning composition |
CN105062712B (en) * | 2015-07-29 | 2018-01-12 | 广州立白企业集团有限公司 | A kind of foam type fruits and vegetables dish washing detergent compositions |
EP4382592A1 (en) * | 2022-12-06 | 2024-06-12 | The Procter & Gamble Company | Water-soluble unit dose article comprising a fibrous non-woven sheet and a surfactant system |
EP4382590A1 (en) * | 2022-12-06 | 2024-06-12 | The Procter & Gamble Company | A process for making a magnesium linear alkyl benzene sulphonate anionic detersive surfactant flake |
Family Cites Families (3)
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US3703772A (en) * | 1971-07-27 | 1972-11-28 | Colgate Palmolive Co | Drying of detergents |
GB1437950A (en) * | 1972-08-22 | 1976-06-03 | Unilever Ltd | Detergent compositions |
EP0135920B1 (en) | 1983-09-22 | 1987-08-26 | Dresser Industries,Inc. | Improved process for making alkaline-earth metal salts of alkaryl sulfonic acids |
-
2007
- 2007-07-27 EP EP07113313A patent/EP1967512A3/en not_active Withdrawn
-
2008
- 2008-03-05 CN CN200880007527A patent/CN101627010A/en active Pending
- 2008-03-05 EP EP08717440A patent/EP2121588A2/en not_active Withdrawn
- 2008-03-05 BR BRPI0808550-1A2A patent/BRPI0808550A2/en not_active IP Right Cessation
- 2008-03-05 WO PCT/EP2008/052692 patent/WO2008107463A2/en active Search and Examination
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See references of WO2008107463A2 * |
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BRPI0808550A2 (en) | 2014-08-19 |
EP1967512A2 (en) | 2008-09-10 |
EP1967512A3 (en) | 2009-07-01 |
WO2008107463A2 (en) | 2008-09-12 |
CN101627010A (en) | 2010-01-13 |
WO2008107463A3 (en) | 2009-08-06 |
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