EP0060587A2 - Agglomerierungsverfahren zur Herstellung von körnigen Reinigungsmitteln - Google Patents
Agglomerierungsverfahren zur Herstellung von körnigen Reinigungsmitteln Download PDFInfo
- Publication number
- EP0060587A2 EP0060587A2 EP82200251A EP82200251A EP0060587A2 EP 0060587 A2 EP0060587 A2 EP 0060587A2 EP 82200251 A EP82200251 A EP 82200251A EP 82200251 A EP82200251 A EP 82200251A EP 0060587 A2 EP0060587 A2 EP 0060587A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- alkali metal
- process according
- added
- particulate components
- dispenser cup
- 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.)
- Granted
Links
- 239000003599 detergent Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims description 29
- 230000008569 process Effects 0.000 title claims description 24
- 238000005054 agglomeration Methods 0.000 title description 3
- 230000002776 aggregation Effects 0.000 title description 3
- 239000000203 mixture Substances 0.000 claims abstract description 53
- 235000019832 sodium triphosphate Nutrition 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 10
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims abstract description 6
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 16
- 239000007859 condensation product Substances 0.000 claims description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 239000003112 inhibitor Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims description 11
- 239000002736 nonionic surfactant Substances 0.000 claims description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 9
- 239000000460 chlorine Substances 0.000 claims description 9
- 229910052801 chlorine Inorganic materials 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 150000001340 alkali metals Chemical class 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 7
- 238000005187 foaming Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 150000004665 fatty acids Chemical class 0.000 claims description 4
- 125000002252 acyl group Chemical group 0.000 claims description 2
- 125000002947 alkylene group Chemical group 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 abstract description 10
- 239000004115 Sodium Silicate Substances 0.000 abstract description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052911 sodium silicate Inorganic materials 0.000 abstract description 9
- 239000000243 solution Substances 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- -1 alkali metal salts Chemical class 0.000 description 10
- 229910052681 coesite Inorganic materials 0.000 description 8
- 229910052906 cristobalite Inorganic materials 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 229910052682 stishovite Inorganic materials 0.000 description 8
- 229910052905 tridymite Inorganic materials 0.000 description 8
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 7
- 230000036571 hydration Effects 0.000 description 6
- 238000006703 hydration reaction Methods 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 5
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 235000021317 phosphate Nutrition 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 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 3
- 229920000388 Polyphosphate Polymers 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 3
- 150000008041 alkali metal carbonates Chemical class 0.000 description 3
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 3
- 238000004851 dishwashing Methods 0.000 description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 3
- 239000001205 polyphosphate Substances 0.000 description 3
- 235000011176 polyphosphates Nutrition 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 159000000001 potassium salts Chemical class 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000003760 tallow Substances 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical class [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- FDIPWBUDOCPIMH-UHFFFAOYSA-N 2-decylphenol Chemical compound CCCCCCCCCCC1=CC=CC=C1O FDIPWBUDOCPIMH-UHFFFAOYSA-N 0.000 description 1
- CYEJMVLDXAUOPN-UHFFFAOYSA-N 2-dodecylphenol Chemical compound CCCCCCCCCCCCC1=CC=CC=C1O CYEJMVLDXAUOPN-UHFFFAOYSA-N 0.000 description 1
- JOONSONEBWTBLT-UHFFFAOYSA-N 2-tetradecylphenol Chemical compound CCCCCCCCCCCCCCC1=CC=CC=C1O JOONSONEBWTBLT-UHFFFAOYSA-N 0.000 description 1
- DHURZBNESRVDPJ-UHFFFAOYSA-N 4-heptadecylphenol Chemical compound CCCCCCCCCCCCCCCCCC1=CC=C(O)C=C1 DHURZBNESRVDPJ-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910019093 NaOCl Inorganic materials 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000004645 aluminates Chemical class 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
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 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
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 159000000011 group IA salts Chemical class 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical class OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 125000000963 oxybis(methylene) group Chemical group [H]C([H])(*)OC([H])([H])* 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920001983 poloxamer Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- IFIDXBCRSWOUSB-UHFFFAOYSA-M potassium;1,5-dichloro-4,6-dioxo-1,3,5-triazin-2-olate Chemical compound [K+].ClN1C(=O)[N-]C(=O)N(Cl)C1=O IFIDXBCRSWOUSB-UHFFFAOYSA-M 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- WTGQALLALWYDJH-WYHSTMEOSA-N scopolamine hydrobromide Chemical compound Br.C1([C@@H](CO)C(=O)OC2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 WTGQALLALWYDJH-WYHSTMEOSA-N 0.000 description 1
- 150000004666 short chain fatty acids Chemical class 0.000 description 1
- 235000021391 short chain fatty acids Nutrition 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical group [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 238000004448 titration Methods 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
- C11D3/06—Phosphates, including polyphosphates
- C11D3/062—Special methods concerning phosphates
-
- 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
- C11D1/66—Non-ionic compounds
- C11D1/72—Ethers of polyoxyalkylene glycols
-
- 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
Definitions
- This invention relates to a process for making a granular detergent product and the product of the process. More particularly, the invention relates to a process for preparing detergent compositions which are useful in automatic dishwashing machines.
- compositions comprising in combination an alkali metal polyphosphate such as sodium tripolyphosphate, alkaline salts such as sodium silicate and sodium carbonate, a surfactant and a chlorine containing compound that provides hypochlorite ion in solution have particular utility for machine dishwashing.
- alkali metal polyphosphate such as sodium tripolyphosphate
- alkaline salts such as sodium silicate and sodium carbonate
- a surfactant and a chlorine containing compound that provides hypochlorite ion in solution
- a chlorine containing compound that provides hypochlorite ion in solution
- U.S. Patent 2,895,916 discloses an order of addition in which chlorinated trisodium phosphate is added to the composition only after the aqueous silicate has been added to an anhydrous polyphosphate. A carton caking benefit is said-to result from a more rapid hydration of the sodium tripolyphosphate in the absence of chlorinated trisodium phosphate.
- 20% of certain alkali metal salts are added to the detergent composition after the agglomeration step comprising the addition of water or an aqueous alkali metal silicate solution to a particulate mixture comprising sodium tripolyphosphate has commenced and preferably is substantially complete.
- agglomerated granular detergent composition comprising from 15% to 50% of sodium tripolyphosphate, from 5% to 25% silicate solids wherein the average SiO 2 :M 2 O weight ratio is from 1.0 to 3.6, M being an alkali metal, from 2% to 12% of a low-foaming nonionic surfactant and from 2% to 20% of alkali metal chlorides and mixtures thereof, wherein the said agglomerated granular detergent composition is prepared by agitating particulate components comprising anhydrous sodium tripolyphosphate, contacting said particulate components during said agitation with an agglomerating agent comprising water, mixing said agglomerating agent with said particulate components by continuing said agitation, adding a dispenser cup caking inhibitor during said agitation after at least 30% of said agglomerating agent has been added to said particulate components, said dispenser cup caking inhibitor comprising said one or more alkali metal chlorides and being a dry
- the process of the invention is carried out in apparatus suitable. for the mixing of dry particulate components and adapted so that liquid components such as water or an aqueous alkali metal silicate solution agglomerating agent can be sprayed on or otherwise added to a bed or falling curtain of one or more particulate components during the mixing operation.
- Any suitable mixing device such as an inclined pan aggldmerator, a rotating drum or any other vessel with suitable means of agitation may be used. Methods of agitating, mixing and agglomerating particulate components are well known to those skilled in the art.
- the apparatus may be designed or adapted for either continuous or batch operation so long as the essential process steps can be achieved.
- Optional process steps include screening of particulate materials before processing, screening or grinding the composition to any desired particle size, addition of optional ingredients such as an alkali metal dichlorocyanurate bleach and sodium carbonate, and allowing the final composition to come to equilibrium with respect to temperature and hydration before packing into cartons.
- optional ingredients such as an alkali metal dichlorocyanurate bleach and sodium carbonate
- the theoretical basis for the unexpected improvement in dispenser cup caking resistance provided by incorporation of the dispenser cup caking inhibitor is believed to be at least partially related to the complex hydration characteristics of anhydrous sodium tripolyphosphate.
- This compound has different hydration characteristics depending on its method of manufacture.
- a so-called Form I is produced if the process of manufacture includes a relatively high temperature calcination step.
- a Form II results when lower temperatures are employed.
- Form I is characterized by relatively rapid hydration characteristics.
- Form II particularly in the absence of any substantial level of Form I material, is slow to hydrate, but has a greater immediate solubility.
- Commercially available sodium tripolyphosphate is generally a mixture of Form I and Form II.
- U.S. Patents 2,622,068, 2,961,409 and 2,961,410 disclose the hydration characteristics of Form I and Form II sodium tripolyphosphate in the manufacture of spray-dried detergents.
- the process and product of this invention apply to granular detergent compositions comprising the following essential ingredients: (1) sodium tripolyphosphate; (2) alkali metal silicate; (3) a low-foaming nonionic surfactant; and (4) an alkali metal salt dispenser cup caking inhibitor.
- the detergent compositions of the invention contain sodium tripolyphosphate at a level of from 15% to 50% and preferably from 25% to 45% by weight.
- Anhydrous sodium tripolyphosphate comprises. all or a part of the particulate components contacted with the agglomerating agent in the process aspect. of the invention.
- the sodium tripolyphosphate can be in granular form such that at least 90% is retained on a 100 Tyler mesh screen or in powdered form such that at least 90% passes through a 100 Tyler mesh sereen.
- Optional polyphosphates useful in the practice of the invention are the water-soluble sodium and potassium salts of pyrophosphoric acid (H 4 P 2 O 7 ) and polymeric metaphosphoric acid (HP0 3 )n.
- the value of n is typically below - 50 in the interest of water solubility.
- the sodium and potassium salts of metaphosphoric acid are often designated "glassy" phosphates and exist as a series of polymers. Glassy phosphates may also be represented by the formula (M 2 0)m(P 2 0 5 )n wherein M is an alkali metal, n is in the range of from 5 to 50 and m:n is in the range of 1:1 to 1:1.5 on a molar basis.
- An example of a glassy phosphate is sodium hexametaphosphate (Na 6 P 6 O 18 ).
- compositions made by the process of this invention contain alkali metal silicate solids at a level of from 5% to 25% on an anhydrous weight basis and having an average Si0 2 :M 2 0 weight ratio of from 1.0 to - 3.6, M being an alkali metal.
- a sodium silicate having a weight ratio of Si0 2 :Na 2 0 of from 1.6 to 3.3, most preferably from
- Aqueous alkali metal silicate solutions used as agglomerating agents preferably contain at least 45% water.
- Silicate solids in the compositions of the invention can be added dry in anhydrous or hydrous form.
- Preferably at least a' portion of the total silicate is hydrous silicate mixed with sodium tripolyphosphate before the addition of an agglomeration agent.
- compositions of this invention contain from 2.0% to 12% of a low-foaming nonionic surfactant by weight.
- a preferred level of surfactant is from 3.0% to 8.0%.
- the surfactant is an alkoxylated nonionic surfactant and preferably the composition is essentially free of sulfonated or sulfated anionic surfactants.
- nonionic surfactants examples include:
- Preferred surfactants are those having the formula RO-(C 2 H 4 O) x R 1 wherein R is an alkyl or alkylene group containing from 17 to 19 carbon atoms, x is a number from 6 to
- R is selected from hydrogen, C l-5 alkyl groups, C 2-5 acyl groups and groups having the formula -(C y H 2y O) n H wherein y is 3 to 4 and n is a number from 1 to 4.
- low sudsing compounds of (4), the other compounds of (5), and C 17-19 materials of (1) which have a narrow ethoxy distribution.
- compositions of the invention contain from 2% to 20%, preferably from 4% to 15%, of a dispenser cup caking inhibitor selected from alkali metal chlorides and mixtures thereof.
- Operative dispenser cup caking inhibitors are in the form of dry powders having a particle size such that at least 80% passes through a 35 Tyler mesh screen (mesh size 0.422 mm).
- the dispenser cup caking inhibitor is added during the process of the invention after at least 30%, preferably 75%, and most preferably 90%, of the water or aqueous sodium silicate agglomerating agent has been added to the particulate components comprising sodium tripolyphosphate.
- An especially preferred material is sodium chloride having a particle size such that at least 80% passes through a 100 Tyler mesh screen (mesh size 0.152 mm).
- compositions of the invention are made by a process in which either water or an aqueous sodium silicate solution is used as the agglomerating agent.
- the finished compositions will contain water in the form of hydrated salts, preferably from 9% to 12% by weight.
- Sodium or potassium dichlorocyanurate is optionally but preferably incorporated in the compositions of the invention in an amount sufficient to provide available chlorine equal to from 0.75% to 2.5% by weight of the composition.
- a preferred material is sodium dichlorocyanurate dihydrate as disclosed in U.S. Patent 3,936,386, which provides 56% available chlorine by weight.
- available chlorine The ability of a compound to provide hypochlorite ion in solution is generally measured as "available chlorine".
- the available chlorine reflects the method of producing an inorganic hypochlorite (e.g., 2 NaOH + Cl 2 ⁇ - NaOCl + NaCl + H20).
- Available chlorine is the chlorine liberated by acidification of a solution of hypochlorite ions and at least a molar equivalent amount of chloride ions.
- the usual analytical method of determining available chlorine in a solution is addition of an excess of an iodide salt and titration of the liberated free iodine with a reducing agent.
- the process and composition of the invention utilize alkali metal carbonate to provide the alkalinity needed for optimum cleaning performance.
- Alkali metal carbonates particularly sodium carbonate
- the product sudses too much, to incorporate one of the many suds-suppressing ingredients disclosed in the above mentioned patents at a level of from 0.01% to 10%, preferably from 0.05% to 3%.
- the preferred suds suppressing materials are mono- and distearyl acid phosphates; the self-emulsified siloxane suds suppressors of U.S. Patent 4,126,045, and mixtures thereof.
- Organic sequestering builders such as citrates and nitrilotriacetates can be present in the compositions, but preferably at levels no greater than 10% by weight. The presence.of organic builders tends to hurt the performance of these compositions by leaving visible spots and filming on glassware.
- China protecting agents including aluminosilicates, aluminates, etc., can be present in amounts up to 5%, preferably from 0.2% to 2%.
- Filler materials sodium sulfate in particular, to control product density and other physical characteristics can also be present in amounts up to 60%, preferably not more than 30% by weight.
- Dyes, perfumes, crystal modifiers and the like can also be added in minor amounts.
- compositions were packed in airtight containers pending evaluation. Resistance to automatic dishwasher dispenser cup caking was measured as indicated in the table below.
- Composition A was superior to Composition B in resistance to dispenser cup caking. No Composition A remained in the dispenser cup at the end of the rinse cycle, the point of principal notice of dispenser cup caking.
- Example I-A The process of Example I-A was repeated with the substitution of NaCl having a particle size such that 80% passed through a 35 Tyler mesh screen (mesh size 0.422 mm) and less than 20% passed through a 100 Tyler mesh screen (mesh size 0.152 mm).
- the resultant composition was superior to Composition B of Example I but slightly inferior to Composition A of Example I.
- composition B of Example I The materials listed in the table below were added to Composition B of Example I at the levels and process cycle time indicated. 300 grams of each resultant composition was mixed with 100 grams of 37°C distilled water and stirred in a 400 ml beaker. Viscosity of the product slurries was measured by a Brookfield spindle viscometer (No.4 spindle/6 rpm) after seven minutes.
- All dispenser cup caking inhibitor materials listed above had a particle size such that at least 80% by weight passed through a 100 Tyler mesh screen (mesh size 0.152 mm) except granular NaCl for which 80% passes through a 35 Tyler mesh screen (mesh size 0.422 mm) and 50% is retained on a 65 Tyler mesh screen (mesh size 0.211 mm).
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- 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)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US24328181A | 1981-03-13 | 1981-03-13 | |
US243281 | 1981-03-13 |
Publications (3)
Publication Number | Publication Date |
---|---|
EP0060587A2 true EP0060587A2 (de) | 1982-09-22 |
EP0060587A3 EP0060587A3 (en) | 1983-06-29 |
EP0060587B1 EP0060587B1 (de) | 1986-07-02 |
Family
ID=22918109
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP19820200251 Expired EP0060587B1 (de) | 1981-03-13 | 1982-03-01 | Agglomerierungsverfahren zur Herstellung von körnigen Reinigungsmitteln |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP0060587B1 (de) |
CA (1) | CA1173323A (de) |
DE (1) | DE3271854D1 (de) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999036495A1 (de) * | 1998-01-14 | 1999-07-22 | Cognis Deutschland Gmbh | Homogene tensidgranulate für die herstellung von stückigen wasch- und reinigungsmitteln |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4169806A (en) * | 1978-08-09 | 1979-10-02 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
DE2925137A1 (de) * | 1979-06-22 | 1981-01-08 | Keri Dipl Ing Karoly | Homogene, staubfreie und rieselfaehige wasch- und reinigungsmittelgranulate, sowie verfahren zu deren herstellung |
-
1982
- 1982-03-01 DE DE8282200251T patent/DE3271854D1/de not_active Expired
- 1982-03-01 EP EP19820200251 patent/EP0060587B1/de not_active Expired
- 1982-03-12 CA CA000398237A patent/CA1173323A/en not_active Expired
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4169806A (en) * | 1978-08-09 | 1979-10-02 | The Procter & Gamble Company | Agglomeration process for making granular detergents |
DE2925137A1 (de) * | 1979-06-22 | 1981-01-08 | Keri Dipl Ing Karoly | Homogene, staubfreie und rieselfaehige wasch- und reinigungsmittelgranulate, sowie verfahren zu deren herstellung |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999036495A1 (de) * | 1998-01-14 | 1999-07-22 | Cognis Deutschland Gmbh | Homogene tensidgranulate für die herstellung von stückigen wasch- und reinigungsmitteln |
Also Published As
Publication number | Publication date |
---|---|
EP0060587B1 (de) | 1986-07-02 |
CA1173323A (en) | 1984-08-28 |
DE3271854D1 (en) | 1986-08-07 |
EP0060587A3 (en) | 1983-06-29 |
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