WO1993021297A1 - Procede de fabrication d'un agent de lavage se presentant sous forme de granules et contenant du perborate - Google Patents
Procede de fabrication d'un agent de lavage se presentant sous forme de granules et contenant du perborate Download PDFInfo
- Publication number
- WO1993021297A1 WO1993021297A1 PCT/EP1993/000795 EP9300795W WO9321297A1 WO 1993021297 A1 WO1993021297 A1 WO 1993021297A1 EP 9300795 W EP9300795 W EP 9300795W WO 9321297 A1 WO9321297 A1 WO 9321297A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- weight
- parts
- water
- granulation
- sodium
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 title claims abstract description 16
- 238000005469 granulation Methods 0.000 claims abstract description 31
- 230000003179 granulation Effects 0.000 claims abstract description 31
- 150000003839 salts Chemical class 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 50
- 239000008187 granular material Substances 0.000 claims description 22
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 22
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 18
- 239000004115 Sodium Silicate Substances 0.000 claims description 18
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 239000012459 cleaning agent Substances 0.000 claims description 16
- 239000003599 detergent Substances 0.000 claims description 15
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 15
- XSVSPKKXQGNHMD-UHFFFAOYSA-N 5-bromo-3-methyl-1,2-thiazole Chemical compound CC=1C=C(Br)SN=1 XSVSPKKXQGNHMD-UHFFFAOYSA-N 0.000 claims description 10
- 229910021536 Zeolite Inorganic materials 0.000 claims description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 239000010457 zeolite Substances 0.000 claims description 10
- 239000002736 nonionic surfactant Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 235000019353 potassium silicate Nutrition 0.000 claims description 5
- 159000000000 sodium salts Chemical class 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000006260 foam Substances 0.000 claims description 4
- 150000004687 hexahydrates Chemical class 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 2
- -1 sodium metasilicate hydrates Chemical class 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims 1
- 239000012418 sodium perborate tetrahydrate Substances 0.000 claims 1
- IBDSNZLUHYKHQP-UHFFFAOYSA-N sodium;3-oxidodioxaborirane;tetrahydrate Chemical compound O.O.O.O.[Na+].[O-]B1OO1 IBDSNZLUHYKHQP-UHFFFAOYSA-N 0.000 claims 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 15
- 235000019832 sodium triphosphate Nutrition 0.000 description 14
- 238000003860 storage Methods 0.000 description 14
- 239000001226 triphosphate Substances 0.000 description 14
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 description 13
- 238000004140 cleaning Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 238000004061 bleaching Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000000428 dust Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 150000004682 monohydrates Chemical class 0.000 description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 description 6
- 238000002474 experimental method 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
- 241001122767 Theaceae Species 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- PNBRHWVSGHFKKX-UHFFFAOYSA-N tetrasodium;silicate;pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])[O-] PNBRHWVSGHFKKX-UHFFFAOYSA-N 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 239000005662 Paraffin oil Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000002304 perfume Substances 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 229960001922 sodium perborate Drugs 0.000 description 3
- YKLJGMBLPUQQOI-UHFFFAOYSA-M sodium;oxidooxy(oxo)borane Chemical compound [Na+].[O-]OB=O YKLJGMBLPUQQOI-UHFFFAOYSA-M 0.000 description 3
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical group CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical group OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 2
- 239000011363 dried mixture Substances 0.000 description 2
- 238000007580 dry-mixing Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002191 fatty alcohols Chemical class 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000008233 hard water Substances 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- 150000004686 pentahydrates Chemical class 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000005070 ripening Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 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 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 125000004036 acetal group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 description 1
- 229940018557 citraconic acid Drugs 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008139 complexing agent Substances 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
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 238000007046 ethoxylation reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229940057995 liquid paraffin Drugs 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000008234 soft water Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 235000011178 triphosphate Nutrition 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing 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
- C11D3/08—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
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
- C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/128—Aluminium silicates, e.g. zeolites
-
- 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
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/3757—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions
- C11D3/3761—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions in solid 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
- C11D3/39—Organic or inorganic per-compounds
- C11D3/3942—Inorganic per-compounds
Definitions
- the invention relates to a method for producing a cleaning agent which can be used in dishwashers and which contains a perborate salt as an oxygen carrier.
- German Offenlegungsschrift 29 25 137 proposes homogeneous dust-free and free-flowing detergent and cleaning agent granules which contain pentasodium triphosphate, sodium sulfate, sodium perborate, detergent substances, silicates and complexing agents.
- the constituents are granulated in a reactor at reaction times between 0.1 to 20 seconds and at temperatures below 95 ° C., preferably below 50 ° C., with the addition of water.
- perborate salts are sensitive to water and / or temperatures.
- the pentasodium triphosphate can form salts containing water of crystallization and thus consume the water required for granulation to form the hexahydrate, so that it cannot damage the perborate salts.
- German patent application DE 39 10569 it is proposed to first convert pentasodium triphosphate partially into the hexahydrate to produce a detergent granulate, then to mix it with essentially anhydrous sodium metasilicate, anhydrous sodium carbonate and sodium metasilicate hydrate, to granulate with a water glass solution and then to granulate it , ie not during or before granulation, if necessary add an active oxygen carrier. Finally, the granules obtained in this way should ripen in a moist air stream.
- pentasodium triphosphate is also used, it is possible to granulate perborate salts directly.
- the invention thus relates to a method for producing a cleaning agent for dishwashers with a perborate salt as an oxygen carrier, in which, for example, in a first granulation stage (A)
- anhydrous sodium carbonate of which up to about 5 parts by weight can be replaced by sodium metasilicate hydrates (penta- or hexahydrate), mixed (B) and then in a granulation mixer in a final granulation stage (C)
- the granulation process according to the invention provides for the water softener to be subjected to pregranulation in a first granulation stage.
- water softeners within the meaning of the invention are preferably understood to mean water softeners or water softener combinations free of pentasodium triphosphate.
- about 4 to 25% by weight of the sodium salt of a polycarboxylic acid can be used as the water softener in the first stage.
- the polycarboxylic acid sodium salts in question here are well known to the person skilled in the art.
- They are homopolymers or copolymers of unsaturated monocarboxylic acids or dicarboxylic acids, that is to say in particular one or more monomers from the following group: acrylic acid, methacrylic acid, maleic acid, itaconic acid, citraconic acid.
- Preferred products are in the molecular weight range below 100,000, for example between 50,000 and 70,000.
- the copolymers of acrylic acid and maleic acid in a molar ratio of about 1: 9 to 9: 1 are particularly preferred.
- mixtures of about 10 to 30% by weight of zeolite NaA powder and about 1 to 8% by weight of the sodium salt of one of the aforementioned polycarboxylic acids can be used as the water softener.
- the zeolite NaA powder is the water-containing form customary for use in detergents and cleaning agents, not the annealed water-free form. About 0.1 to 10 parts by weight of water are added for the purpose of granulation, ie the caking of the particles. The water can be added directly as such into the mixing kettle * . In addition to or instead of water can be used but also water-containing surfactant r Zeolithaufschlämmungen.
- Such zeolite slurries are known from the spray drying technology of detergents. They usually consist of about 10 to 60% by weight of zeolite NaA powder, water and nonionic surfactants for stabilization. Suitable nonionic surfactants are, for example, the ethoxylates of long-chain alcohols. Such zeolite slurries are preferably used in an amount of about 2 to 5% by weight.
- the percentage by weight refers here, as elsewhere, to the entire cleaning agent.
- the individual constituents of the cleaning agents are to be selected from the amounts stated so that they total 100% by weight.
- the granulation process is carried out until about 85% by weight of the powder has a grain size of more than 0.2 mm.
- Fast-running mixers and dwell times of 0.2 to 10 seconds are required for this, and the precise setting of these values is easily possible for the cleaning agent technician on the basis of a few preliminary tests.
- Relevant for the grain size of the product of the first stage are, in addition to the amount of water added, in particular the shear forces exerted on the material in the first mixing stage. These shear forces are determined by the number, shape and number of revolutions of the mixing tools arranged in the first mixing stage.
- the number of revolutions of the shaft suitable for the optimal grain distribution, " _T the number of knives and their angle of inclination can easily be determined by the skilled person through experiments.
- the material leaving the first pelletizing stage expediently enters a conveyor device, which in the simplest case consists of a conveyor belt.
- the conveying path and the conveying speed are matched to one another such that the time from leaving the first mixing stage to entering the second stage takes about 10 to at most 60 seconds, preferably about 10 to 30 seconds. It is also advantageous if care is taken to ensure that the water does not evaporate from the material. This can be done by moving the conveyor belt in an atmosphere saturated with water vapor or by overlaying the water softener with the powdered sodium silicate (preferably metasilicate with the above-mentioned S1O2 to Na2 ⁇ ratio).
- a crusher is expediently arranged, which breaks the so-called rollover. H. coarse grains or chunks, crushed.
- anhydrous sodium carbonate (soda) and the sodium metasilicate hydrate which may be used are continuously fed in the intended amount onto the conveyor belt. It is preferred to add these components after the anhydrous metasilicate.
- the anhydrous sodium carbonate to be used should predominantly have a grain size of 0.05 to 1 mm.
- the sodium metasilicate should have an average grain size of 0.2 to 1.5 mm, the amount is 5 to 20 parts by weight or% by weight.
- the mixture reaches a mixer in which the water softener is intimately mixed with the overlaid metasilicate, the soda and the metasilicate hydrate.
- the dry mixing of the components takes about 20 to 120 seconds. Any further heating of the material is stopped by the mixing process. A partial evaporation of the remaining water • f and a lump formation is successfully countered. Particularly good powder properties and favorable granulation conditions are achieved when the dry mixture has a temperature of 45 to 70 ° C.
- the powdery mixture is after the completion of the dry mixing, i.e. H. after complete homogenization, fed to the new granulation.
- This can either be carried out in the same mixing unit if it has the facilities required for the granulation, or it can be a special one.
- Granulator can be used.
- the granulator consists, for example, of a drum mixer which is arranged horizontally or is slightly inclined. It can be rotatably mounted as a whole and equipped with chicanes, or it can also be stationary and equipped with mixing and conveying elements, so-called plow blades, arranged on a rotatable longitudinal shaft. A plurality of nozzles are arranged in the interior of the mixer, by means of which liquid components are sprayed uniformly onto the material whirled around or which trickles down from rotating mixing tools.
- the powdery mixture is sprayed with the aqueous solution of about 0.5 to 5 parts by weight of water glass, dissolved in about 1 to 8 parts by weight of water.
- the aqueous solution of about 0.5 to 5 parts by weight of water glass, dissolved in about 1 to 8 parts by weight of water.
- about 2 to 15 parts by weight of perborate salt are added.
- Sodium perborate which can be present as a monohydrate or pentahydrate, is preferred.
- a foam inhibitor e.g. B. a liquid paraffin oil or a liquid silicone oil to be added
- this can be injected before the aqueous silicate solution. Amounts of about 1 to 3 parts by weight are preferred. It is also advantageous to spray the nonionic, low-foaming surfactant to be added in an amount of from 0 to about 3 parts by weight (preferably about 0.5 to 3 parts by weight) in the final granulation step. This can be done together with the sodium silicate solution or separately from it via a separate spray nozzle. However, the surfactant can also be mixed in at a later point in the process, with any small amounts of dust present in the finished granulated product being bound respectively • ⁇ - be glued to the granulate.
- the known ethoxylation products of long-chain alcohols and alkylphenols are suitable as nonionic surfactants, the free hydroxyl group of the polyethylene glycol ether residue being substituted by ether or acetal groups or by polypropylene glycol ether residues or butyl ether residues to reduce the tendency to foam.
- the block polymers of ethylene oxide with polypropylene oxide or also the alkyl polyglycosides are also suitable.
- the average residence time in the granulation stage is generally about 60 to 300 seconds, preferably about 90 to 200 seconds.
- the granulation mixer can be operated continuously or in batches.
- the material emerging from the granulation mixer generally has a temperature of about 55 to 88 ° C. and still requires a short ripening or recrystallization time of about 5 to a maximum of 15 minutes, usually of about 3 to 12 minutes, during which it is used Avoiding clump formation is kept in motion.
- the very sensitive perboate salt can be processed under the specified conditions with no or no significant loss of activity.
- the completely crystallized, ripened granulate can be processed further in a manner known per se after leaving the vortex channel, that is, if not yet done, cooled with flowing air and, if desired, mixed with other constituents of the detergent, such as dyes, etc.
- the granules are largely resistant to abrasion and have a favorable grain spectrum of approximately 0.2 to 31.5 m, ie. H. their dust content is minimal. It is particularly advantageous that the method of operation according to the invention does not cause caking at any time - for example on container walls and / or mixing elements.
- Coarse grain formed to a small extent can be mixed into the product again after sieving and grinding. Small amounts of dust, which, for example, are swept along by the circulating air when passing through the vortex trough, can be recovered in dust separators and returned to the granulation mixer.
- the granules are easy to pour and scatter, do not tend to separate and are stable in storage. When used, they show faultless flushing behavior, even under unfavorable conditions, ie in not optimally designed flushing devices. -5 examples
- a cleaning agent for use in a household dishwasher was produced.
- the products according to the present invention had approximately the following composition (in% by weight):
- sodium silicate Na2 ⁇ : S ⁇ 2
- paraffin oils 0 to 30%, preferably 0 to 30% sodium carbonate
- the mixer essentially consisted of a vertically arranged downpipe with nozzles arranged in the upper third, pointing downwards, and a central, rotatable shaft on which two knife rings each with 6 knives were arranged, one in the upper and the second in the lower third of the mixing tube.
- the knife planes were inclined up to 5 ° to the horizontal in order to achieve a slight suction effect.
- the speed of the shaft was 2000 to 3000 rpm in the examples.
- the powder fell into an inclined towards the horizontal, from a fixed ⁇ o - tube equipped with rotating agitator and conveying elements mixer (II).
- the average residence time in the mixing zone (B) was approximately 30 seconds at a temperature of approximately 65 ° C.
- the product entered the granulation zone (C), where it was mixed with an aqueous solution of 0.2 part by weight of perfume, 1.5 parts by weight of paraffin oil and 1.3 parts by weight of water glass 3. 0 was sprayed continuously. Then 7.0 parts by weight of sodium perborate monohydrate were added.
- the product was discharged and reached one. vortex channel arranged in a closed chamber. In this vortex channel, air heated to 95 ° C. with a relative humidity of 70 to 80% was circulated.
- the average residence time of the granules in the vortex channel was 10 minutes.
- the product had better bleaching properties compared to tea and coffee stains like comparable composite commercial powder cleaning agents, which may have been due to a lack of homogeneity in powder compositions.
- Example 2 The procedure was the same as in Example 1.
- the zeolite powder was added in step A together with the metasilicate to the moist pentasodium triphosphate.
- the temperature of the material emerging from the granulation mixer was lower than in Example 1 and was approximately 60-70 ° C.
- stage A the hydration phase
- stage B the components for the replacement of phosphate are added to stage B, whereby the material naturally does not heat up in this stage due to the absence of the heat of hydration.
- the sodium perborate monohydrate is then added in the granulation stage (C).
- the temperature of the material emerging from the granulation mixer does not exceed approx. 50 ° C. in the case of the phosphate-free mixtures.
- A2 Sodium orthosilate pentahydrate in the weight ratio of agglomerate to silicate such as about 9: 1 can also be mixed into the agglomerate.
- a phosphate and zeolite-free cleaning agent could also be produced by the process according to the invention. It had the following composition:
- Sodium orthosilicate pentahydrate and nonionic surfactant can also be added to the agglomerate obtained according to the following recipe.
- a raw material mixture consisting of
- sodium perborate monohydrate -3 was granulated with a total of 19.08% by weight of water.
- Sodium perborate monohydrate was added to the wet granules and the mixture was dried in a fluidized bed.
- the temperature of the supply air was 80 ° C in test 1 and 100 ° C in test 2.
- the dried product was with
- Ci2-Ci4 fatty alcohol 1.00% by weight of Ci2-Ci4 fatty alcohol. 4 E0 x 5 PO and 15.00 wt .-% sodium orthosilicate pentahydrate mixed. The final water content of the blended products is 2.98%.
- the cleaning performance was determined with standard soiling. Grade 0 receives the original soiled dishes. A grade of 10 is given with optimal cleaning.
- the standard product is a commercially available cleaner of the following composition:
- This cleaning agent was produced from the individual raw materials by mixing.
- Table 1 Cleaning performance immediately after production of the dishwasher: Miele G 590 program: 55 ° C universal
- Dishwasher Miele G 590 program: 55 ° C universal
- the products with granulated perborate monohydrate were examined under various conditions: room temperature conditions (20 ° C / 50% relative air humidity, 30 ° C / 80% relative air humidity, 40 ° C).
- the most important parameters for the products with granulated perborate monohydrate are the active oxygen content and the cleaning performance in the case of tea stains.
- the bleaching performance of tea stains correlates with the active oxygen content of the product.
- the cleaning performance was confirmed under hard water conditions (16 ° d) in order to clearly work out differences in performance in tea bleaching.
- a bleaching performance of notes 3 - 4 under hard water conditions (16 ° d) corresponds to notes 7 - 9 under soft water conditions (softened water).
- Water softening is state of the art in dishwashers.
- the bleaching performance of the products with granulated perborate monohydrate is sufficient for good bleaching performance even after storage under the conditions mentioned above.
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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)
Abstract
L'invention concerne un procédé de fabrication d'un agent de lavage pour lave-vaisselle selon lequel on peut utiliser du perborate. Selon ledit procédé, l'on granule le perborate dans une seconde phase de granulation conjointement avec les autres constituants prégranulés et mélangés avec ledit perborate.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP93908873A EP0636168A1 (fr) | 1992-04-10 | 1993-04-01 | Procede de fabrication d'un agent de lavage se presentant sous forme de granules et contenant du perborate |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19924212166 DE4212166A1 (de) | 1992-04-10 | 1992-04-10 | Verfahren zur Herstellung perborathaltiger Reinigergranulate |
DEP4212166.3 | 1992-04-10 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1993021297A1 true WO1993021297A1 (fr) | 1993-10-28 |
Family
ID=6456607
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP1993/000795 WO1993021297A1 (fr) | 1992-04-10 | 1993-04-01 | Procede de fabrication d'un agent de lavage se presentant sous forme de granules et contenant du perborate |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP0636168A1 (fr) |
DE (1) | DE4212166A1 (fr) |
WO (1) | WO1993021297A1 (fr) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1996027650A1 (fr) * | 1995-03-06 | 1996-09-12 | Brunner Mond & Company Limited | Produit granulaire du type agent de blanchiment/adjuvant de detergence |
US5929021A (en) * | 1995-12-20 | 1999-07-27 | Lever Brothers, Division Of Conopco, Inc. | Process for preparing a granular detergent |
US8323945B2 (en) | 2008-06-06 | 2012-12-04 | Danisco Us Inc. | Variant alpha-amylases from Bacillus subtilis and methods of uses, thereof |
US9040278B2 (en) | 2008-06-06 | 2015-05-26 | Danisco Us Inc. | Production of glucose from starch using alpha-amylases from Bacillus subtilis |
US9040279B2 (en) | 2008-06-06 | 2015-05-26 | Danisco Us Inc. | Saccharification enzyme composition and method of saccharification thereof |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
MX2009009378A (es) | 2007-03-09 | 2009-09-22 | Danisco Us Inc Genencor Div | Variantes de alfa-amilasa de especies de bacillus alcalifilico, composiciones que comprenden las variantes de alfa-amilasa, y metodos de uso. |
WO2011049945A2 (fr) | 2009-10-23 | 2011-04-28 | Danisco Us Inc. | Procédés destinés à réduire le saccharide donnant une couleur bleue |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1071874B (fr) * | 1959-12-24 | |||
DE2925137A1 (de) * | 1979-06-22 | 1981-01-08 | Keri Dipl Ing Karoly | Homogene, staubfreie und rieselfaehige wasch- und reinigungsmittelgranulate, sowie verfahren zu deren herstellung |
EP0202519A1 (fr) * | 1985-05-16 | 1986-11-26 | AUSIMONT S.p.A. | Procédé de production de perborate de sodium monohydraté en granulés d'une bonne résistance mécanique |
DE3910569A1 (de) * | 1989-04-01 | 1990-10-04 | Henkel Kgaa | Verfahren zur herstellung eines maschinengeschirrspuelmittel-granulates |
WO1991002696A1 (fr) * | 1989-08-19 | 1991-03-07 | Henkel Kommanditgesellschaft Auf Aktien | Procede de granulation de monohydrate de perborate |
-
1992
- 1992-04-10 DE DE19924212166 patent/DE4212166A1/de not_active Withdrawn
-
1993
- 1993-04-01 WO PCT/EP1993/000795 patent/WO1993021297A1/fr not_active Application Discontinuation
- 1993-04-01 EP EP93908873A patent/EP0636168A1/fr not_active Withdrawn
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1071874B (fr) * | 1959-12-24 | |||
DE2925137A1 (de) * | 1979-06-22 | 1981-01-08 | Keri Dipl Ing Karoly | Homogene, staubfreie und rieselfaehige wasch- und reinigungsmittelgranulate, sowie verfahren zu deren herstellung |
EP0202519A1 (fr) * | 1985-05-16 | 1986-11-26 | AUSIMONT S.p.A. | Procédé de production de perborate de sodium monohydraté en granulés d'une bonne résistance mécanique |
DE3910569A1 (de) * | 1989-04-01 | 1990-10-04 | Henkel Kgaa | Verfahren zur herstellung eines maschinengeschirrspuelmittel-granulates |
WO1991002696A1 (fr) * | 1989-08-19 | 1991-03-07 | Henkel Kommanditgesellschaft Auf Aktien | Procede de granulation de monohydrate de perborate |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1996027650A1 (fr) * | 1995-03-06 | 1996-09-12 | Brunner Mond & Company Limited | Produit granulaire du type agent de blanchiment/adjuvant de detergence |
US5929021A (en) * | 1995-12-20 | 1999-07-27 | Lever Brothers, Division Of Conopco, Inc. | Process for preparing a granular detergent |
US6077820A (en) * | 1995-12-20 | 2000-06-20 | Lever Brothers Company Division Of Conopco, Inc. | Process for preparing a granular detergent |
US8323945B2 (en) | 2008-06-06 | 2012-12-04 | Danisco Us Inc. | Variant alpha-amylases from Bacillus subtilis and methods of uses, thereof |
US8975056B2 (en) | 2008-06-06 | 2015-03-10 | Danisco Us Inc. | Variant alpha-amylases from Bacillus subtilis and methods of uses, thereof |
US9040278B2 (en) | 2008-06-06 | 2015-05-26 | Danisco Us Inc. | Production of glucose from starch using alpha-amylases from Bacillus subtilis |
US9040279B2 (en) | 2008-06-06 | 2015-05-26 | Danisco Us Inc. | Saccharification enzyme composition and method of saccharification thereof |
US9090887B2 (en) | 2008-06-06 | 2015-07-28 | Danisco Us Inc. | Variant alpha-amylases from Bacillus subtilis and methods of use, thereof |
Also Published As
Publication number | Publication date |
---|---|
DE4212166A1 (de) | 1993-10-14 |
EP0636168A1 (fr) | 1995-02-01 |
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