EP2207871B1 - Compositions de lessive ou de détergent et leur fabrication - Google Patents

Compositions de lessive ou de détergent et leur fabrication Download PDF

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Publication number
EP2207871B1
EP2207871B1 EP08842723.2A EP08842723A EP2207871B1 EP 2207871 B1 EP2207871 B1 EP 2207871B1 EP 08842723 A EP08842723 A EP 08842723A EP 2207871 B1 EP2207871 B1 EP 2207871B1
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EP
European Patent Office
Prior art keywords
active substance
cleaning agent
carrier material
detergent
weight
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.)
Not-in-force
Application number
EP08842723.2A
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German (de)
English (en)
Other versions
EP2207871A2 (fr
Inventor
Georg Assmann
Olaf Joachim Blochwitz
Gerhard Blasey
Birgit Burg
Hermann-Josef Welling
Ulrich Pegelow
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel AG and Co KGaA
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Henkel AG and Co KGaA
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Publication date
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Priority to PL08842723T priority Critical patent/PL2207871T3/pl
Publication of EP2207871A2 publication Critical patent/EP2207871A2/fr
Application granted granted Critical
Publication of EP2207871B1 publication Critical patent/EP2207871B1/fr
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082—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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/08—Silicates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—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
    • C11D3/1233—Carbonates, e.g. calcite or dolomite
    • 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
    • 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

Definitions

  • the present invention relates to a granulation process for the preparation of a particulate detergent or detergent compound in a fluidized bed granulator, a detergent or cleaning agent compound comprising a core and at least two trays, and a detergent or cleaning agent in which said detergent or cleaning agent compound is included.
  • the detergent or cleaning agent compound contains at least one active substance and a carrier material selected from the group of amorphous aluminosilicates, clays, silicic acids, alkaline earth metal silicates and alkaline earth metal carbonates.
  • Modern powdered to granular detergents or cleaners contain a variety of washing or cleaning active ingredients, also called active ingredients, which are present in substance in solid, pasty or in liquid form.
  • active ingredients also called active ingredients
  • the task of making up the liquid and pasty components together with the solid constituents of the agent so that the liquid and pasty components during storage, transport and use of the agent by the Consumers do not bleed and it does not lead to sticking within the particulate means or smearing and sticking of the particulate agent to the dosing of the consumer, the inner walls of the packaging or the bottling plants in the manufacturing plant.
  • powdering agents is the possible content of liquid or pasty detergent or cleaning ingredients or the content of those detergent or cleaning agent components, which are usually introduced as a solution or dispersion and thus also in liquid or pasty form in the detergent or cleaning compound , low, or with an increased content of these ingredients, the detergent or cleaning compound compound has poor physical properties such as a high tack and thus a poor flowability and a high tendency to bleed.
  • the present invention is a process according to claim 1 for the preparation of a particulate detergent or detergent compound by granulation of an active at 0 to 100 ° C to pasty active substance preparation with the addition of a solid in a fluidized bed granulator, wherein the solid one or more support materials from the Group of amorphous aluminosilicates, clays, silicas, alkaline earth metal silicates and alkaline earth metal carbonates.
  • Fluidized bed granulators are known in the art, for example, under the designations fluidized bed granulator, fluidized bed mixer, fluidized bed dryer fluidized bed dryer or fluidized bed mixer.
  • particulate solids are flowed through from below by a fluidizing gas and fluidized from a certain speed of the fluidizing gas. It forms the so-called fluidized bed, in which from the so-called vortex point, the gravity of the solid particles is compensated by the resistance to the flow. Achieving this point depends on a number of physical factors such as the density, size, distribution and shape of the particles.
  • fluidizing gas Air, nitrogen or water vapor, as well as a mixture of these and in particular air, is preferably used in processes according to the invention.
  • Corresponding apparatus can be used, for example, for drying or cooling particulate solids.
  • a liquid or pasty active substance preparation is introduced into the fluidized bed and granulated by the intimate turbulence within the fluidized-bed granulator together with the solid contained in the fluidized bed.
  • the feeding of a solid into the fluidized bed granulator is an essential step of the process of the invention.
  • the solid fed into the fluid bed granulator contains one or more support materials from the group of amorphous aluminosilicates, clays, silicic acids, alkaline earth silicates and alkaline earth carbonates.
  • the solid fed into the fluid bed granulator may contain one or more further particulate components.
  • Suitable further particulate components are preferably selected from the group of builders and fillers.
  • the solid preferably contains zeolites, citrates, silicates, carbonates, sulfates and / or polycarboxylates.
  • the use of solid surfactants or surfactant mixtures as part of the solid used in the fluidized bed granulator is also advantageous.
  • Suitable support materials in the context of the present invention are materials which have very good absorption properties.
  • the oil absorption capacity which can be determined according to the standard ISO 787-5. According to this method, a sample amount of the particulate material to be examined is placed on a plate. From a burette is slowly - 4 or 5 drops at once - added dropwise Lackleinöl and rubbed after each addition, the oil with a knife spatula in the particulate material. The addition of the oil is continued accordingly until clumps of solid and oil have formed. From this point, add 1 drop each and rub thoroughly with the knife blade after each addition of oil. When a soft paste is formed, the addition of oil is stopped.
  • the paste should just be spread - without cracking or crumbling - and just stick on the plate.
  • the oil absorption capacity is expressed in ml of oil per 100 g of sample.
  • the carrier material used in the method according to the invention preferably has an oil absorption capacity - quantified by the ISO 787-5 standard - above 40 ml / 100 g, more preferably above 60 ml / 100 g, more preferably above 80 ml / 100 g, more preferably above 100 ml / 100 g, most preferably above 120 ml / 100 g, with preference to above 140 ml / 100 g and in particular above 160 ml / 100 g.
  • the BET surface area (according to DIN 66131) of the carrier material is independent of the values of the oil absorption capacity, preferably at at least 10 m 2 / g, preferably at least 40 m 2 / g, more preferably at least 70 m 2 / g, with preference for this purpose at least 100 m 2 / g and in particular at least 130 m 2 / g.
  • the average particle size d 50 of the support material is below 100 .mu.m, preferably below 75 .mu.m, more preferably below 50 .mu.m, and in particular below 25 .mu.m.
  • the support material preferably contains amorphous aluminosilicates.
  • amorphous aluminosilicates with different proportions of alumina (Al 2 O 3 ) and silicon dioxide (SiO 2 ) are understood to contain other metals.
  • the amorphous aluminosilicate used in the process according to the invention can be described by means of a formula (I) or (II).
  • M represents an alkali metal, preferably sodium or potassium.
  • x takes values from 0.2 to 2.0, y the values from 0.5 to 10.0 and w all positive values including 0. x (M 2 O). Al 2 O 3 .y (SiO 2 ) .w (H 2 O) (I)
  • Me stands for an alkaline earth metal
  • M for an alkali metal
  • x for values of 0.001 to 0.1
  • y for values of 0.2 to 2.0
  • z for values of 0.5 to 10
  • 0 and w for positive values including 0.
  • the support material may preferably comprise bentonites, alkaline earth metal silicates, preferably calcium silicate, alkaline earth metal carbonates, in particular calcium carbonate and / or magnesium carbonate and / or silica.
  • Silicas are particularly preferably contained in the support material, the term silica here as a collective name for compounds of general formula (SiO 2 ) m ⁇ nH 2 O stands.
  • Precipitated silicas are prepared from an aqueous alkali silicate solution by precipitation with mineral acids. This forms colloidal primary particles, which agglomerate with progressive reaction and finally grow into aggregates.
  • the powdery, voluminous forms have BET surface areas of 30 to 800 m 2 / g.
  • the term pyrogenic silicas combines highly disperse silicas which are prepared by flame hydrolysis. In this case, silicon tetrachloride is decomposed in a blast gas flame.
  • Pyrogenic silicic acids have significantly less OH groups on their surface than precipitated silicas. Because of their silanol-related hydrophilicity, the synthetic silicic acids are often subjected to chemical aftertreatment processes. in which the OH groups react, for example, with organic chlorosilanes. This results in modified, eg hydrophobic surfaces, which significantly expand the performance properties of the silicic acids. Also chemically modified silicas fall within the scope of the present invention under the term "silicas".
  • the support material preferably contains finely divided silica, which is understood as meaning a very finely divided silica whose primary particles preferably have an average size between 5 and 40 nm, preferably between 10 and 30 nm and in particular between 15 and 25 nm.
  • Such highly dispersed silicic acids have a very high surface area, with surface values measured according to BET being between 90 and 500, preferably between 150 and 400, m 2 / g being particularly preferred.
  • an active substance preparation which is in liquid to pasty form at temperatures of 0 to 100 ° C, preferably 20 to 80 ° C and in particular 30 to 60 ° C, with the carrier material already described above or from carrier material existing solid mixed.
  • active substance preparations up to a maximum viscosity of 50 Pa.s are referred to as pasty.
  • the active-substance preparation contains at least 10% by weight of solvent or dispersant
  • at least part of the solvent or dispersant is removed during the granulation of the active-substance preparation.
  • the solvent or dispersant is preferably at least partially removed during the granulation.
  • the temperature of the fluidizing gas is preferably in the range from 30 to 260 ° C., preferably from 60 to 230 °, directly before it enters the fluidized bed granulator C, more preferably at 90 to 200 ° C.
  • the fluidized bed which is formed by the fluidized solid particles within the fluidized bed granulator, preferably has a temperature above 50 ° C, preferably above 55 ° C, preferably above 60 ° C, more preferably above 65 ° C. and especially above 70 ° C.
  • the active-substance preparation is preferably fed into the fluidized-bed granulator at a temperature of 20 to 70 ° C., preferably of 30 to 65 ° C., more preferably of 40 to 60 ° C. and in particular of 50 to 55 ° C., and fluidized Particles dosed. Be the liquid components heated before spraying, a higher throughput can be achieved in the inventive method.
  • the temperature of the fluidizing gas immediately before entering the fluidized bed granulator is preferably in the range from 0 to 100 ° C, preferably at 10 to 90 ° C, more preferably at 15 to 80 ° C, more preferably at 20 to 70 ° C and especially at 25 to 60 ° C.
  • the fluidized bed which is formed by the fluidized solid particles within the fluidized bed granulator, preferably has a temperature in the range of 10 to 80 ° C, preferably in the range of 15 to 75 °, preferably in the range of 20 to 70 ° C.
  • the active substance preparation is preferably fed into the fluidized-bed granulator at a temperature of from 10 to 80 ° C., preferably from 12 to 70 ° C., more preferably from 14 to 60 ° C. and in particular from 16 to 55 ° C., and applied to the fluidized particles ,
  • the solvent or dispersant used is preferably water, a nonaqueous solvent, a mixture of several nonaqueous solvents or mixtures of water and nonaqueous solvent (s).
  • Non-aqueous solvents are derived, for example, from the group of monohydric or polyhydric alcohols, alkanolamines or glycol ethers.
  • Solvents can be used which consist of ethanol, n- or i-propanol, butanols, glycol, propane- or butanediol, glycerol, diglycol, propyl- or butyldiglycol, hexylene glycol, ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol propyl ether, ethylene glycol mono-n-butyl ether, diethylene glycol methyl ether , Diethylene glycol ethyl ether, propylene glycol methyl, ethyl or propyl ether, dipropylene glycol monomethyl or ethyl ether, di-isopropylene glycol monomethyl or ethyl ether, methoxy, ethoxy or butoxy triglycol, 1-butoxyethoxy-2-propanol, 3-methyl-3-methoxybutanol , Propylene glycol t-butyl ether
  • the active ingredient composition preferably contains one or more active ingredients from the list of nonionic surfactants, anionic surfactants, cationic surfactants, optical brighteners, phosphonates, bleach activators, polymers and foam inhibitors.
  • nonionic surfactants it is possible to use all nonionic surfactants known to the person skilled in the art. Low-foaming nonionic surfactants are used as preferred surfactants.
  • the active substance preparation contains nonionic surfactants from the group of alkoxylated alcohols.
  • nonionic surfactants are preferably alkoxylated, advantageously ethoxylated, in particular primary alcohols having preferably 8 to 18 carbon atoms and an average of 1 to 12 moles of ethylene oxide (EO) per mole of alcohol used, in which the alcohol radical may linear or preferably methyl branched in the 2-position or linear and methyl-branched radicals in a mixture may contain, as they are usually present in Oxoalkoholresten.
  • EO ethylene oxide
  • nonionic surfactants and alkyl glycosides of the general formula RO (G) x can be used in which R is a primary straight-chain or methyl-branched, especially methyl-branched in the 2-position aliphatic radical having 8 to 22, preferably 12 to 18 carbon atoms and G is the symbol which represents a glycose unit having 5 or 6 C atoms, preferably glucose.
  • the degree of oligomerization x which indicates the distribution of monoglycosides and oligoglycosides, is any number between 1 and 10; preferably x is 1.2 to 1.4.
  • Nonionic surfactants of the amine oxide type for example N-cocoalkyl-N, N-dimethylamine oxide and N-tallowalkyl-N, N-dihydroxyethylamine oxide, and the fatty acid alkanolamides may also be suitable.
  • Preferred active ingredients are primary, secondary and tertiary amines, alkylpropylenediamines, bisaminopropylamines, alkyldimethylamine oxides, alkyldimethylbetaines, amine ethoxylates, alkylpyrrolidones, alkyliminoglycinates, alkyliminopropionates, alkyliminodipropionates, alkylamine oxide ethoxylates.
  • Nonionic surfactants from the group of alkoxylated alcohols particularly preferably from the group of mixed alkoxylated alcohols and in particular from the group of EO / AO / EO nonionic surfactants, or the PO / AO / PO nonionic surfactants, especially the PO / EO / PO nonionic surfactants are particularly preferred.
  • Such PO / EO / PO nonionic surfactants are characterized by good foam control.
  • the preferred object of the present invention is a process for the preparation of a particulate detergent or cleaner compound by granulating a 0 to 100 ° C liquid to pasty active substance preparation containing one or more nonionic surfactant (s) from the group of ethoxylated alcohols, amine oxides and alkyl glycosides and less as 20 wt .-%, in particular less than 10 wt .-% solvent or dispersant, with the admixing of a solid in a fluidized bed granulator, wherein the solid one or more support materials from the group of amorphous aluminosilicates, clays, silicas, alkaline earth metal silicates , Alkaline earth metal carbonates, preferably silica.
  • the active substance preparation also contains 0.1 to 35 wt .-%, preferably 1 to 30 Wt .-%, more preferably 1.5 to 20 wt .-% and in particular 2 to 10 wt .-% soap, wherein the amounts are based on the active ingredient preparation.
  • the detergent or cleaning agent compound preferably contains 45 to 95% by weight, more preferably 50 to 90% by weight and especially 60 to 85% by weight of nonionic surfactant and preferably 1 to 30% by weight, preferably 1, 5 to 25 wt .-%, more preferably 2 to 20 wt .-%, particularly preferably 2.5 to 15 wt .-% and in particular 3 to 10 wt .-% of one or more support materials from the group of amorphous aluminosilicates, clays , Silicic acids, alkaline earth metal silicates, alkaline earth metal carbonates, preferably silicic acid. With particular preference are 3 to 15 wt .-%, more preferably 3.5 to 10 wt .-% and in particular 4 to 8 wt .-% silica in the detergent or cleaning agent compound.
  • an active agent formulation containing amine oxide, soap and alkyl benzene sulfonate is also preferred.
  • alkylbenzenesulfonates can be used as further anionic surfactants of the sulfonate type or sulfates in the active ingredient preparation.
  • the surfactants of the sulfonate type are preferably C 9-13 -alkylbenzenesulfonates, olefinsulfonates, ie mixtures of alkene and hydroxyalkanesulfonates and disulfonates, as are obtained, for example, from C 12-18 -monoolefins having terminal or internal double bonds by sulfonation with gaseous sulfur trioxide and subsequent alkaline or acid hydrolysis of the sulfonation products into consideration.
  • alkanesulfonates which are obtained from C 12-18 alkanes, for example by sulfochlorination or sulfoxidation with subsequent hydrolysis or neutralization.
  • esters of ⁇ -sulfo fatty acids for example the ⁇ -sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids are suitable.
  • anionic surfactants are particularly soaps into consideration.
  • Suitable are saturated fatty acid soaps, such as the salts of lauric acid, myristic acid, palmitic acid, stearic acid, hydrogenated erucic acid and behenic acid, and in particular of natural fatty acids, e.g. Coconut, palm kernel or tallow fatty acids, derived soap mixtures.
  • the anionic surfactants may be in the form of their sodium, potassium or ammonium salts and as soluble salts of organic bases, such as mono-, di- or triethanolamine.
  • the anionic surfactants are preferably present in the form of their sodium or potassium salts, in particular in the form of the sodium salts.
  • Another preferred subject matter of the present invention is a process for the preparation of a particulate detergent or cleaning agent compound by granulation of an active substance preparation which is liquid to pasty at from 10 to 100 ° C. and which comprises one or more anionic surfactants the group of alkylbenzenesulfonates, fatty alcohol sulfates and ester sulfonates and 20 to 65 wt .-% solvent or dispersant, especially water, with admixture of a solid in a fluidized bed granulator, wherein the solid one or more support materials from the group of amorphous aluminosilicates, clays , Silicas, alkaline earth metal silicates, alkaline earth metal carbonates, preferably containing silica.
  • the detergent or cleaning agent compound preferably contains 45 to 95 wt .-%, with preference to 50 to 90 wt .-% and in particular 55 to 85 wt .-% anionic surfactant and preferably 2 to 20 wt .-%, with preference to 2 bis 15 wt .-% and in particular 2 to 12 wt .-% of one or more support materials from the group of amorphous aluminosilicates, clays, silicic acids, alkaline earth metal silicates, alkaline earth metal carbonates, preferably silica and with particular preference 1 to 10 wt .-%, in particular 2 to 8 wt .-% phosphonate and / or polymer, in particular polycarboxylate.
  • Textile softening compounds can be used to care for the textiles and to improve the textile properties such as a softer "avivage” and reduced electrostatic charging (increased wearing comfort)
  • the active ingredients of these formulations are quaternary ammonium compounds having two hydrophobic radicals, such as the disteraryldimethylammonium chloride
  • quaternary ammonium compounds containing ester groups in their hydrophobic residues as predetermined breaking points for biodegradation.
  • esters with improved biodegradability are obtainable, for example, by esterifying mixtures of methyldiethanolamine and / or triethanolamine with fatty acids and then quaternizing the reaction products in a manner known per se with alkylating agents. Further suitable as a finish is dimethylolethyleneurea.
  • Optical brighteners can be used in the active ingredient preparation in order to eliminate graying and yellowing of the treated textiles. These fabrics impinge on the fiber and cause whitening and bleaching by transforming invisible ultraviolet radiation into visible longer wavelength light, emitting the ultraviolet light absorbed from the sunlight as faint bluish fluorescence, and pure with the yellowness of the grayed or yellowed wash White results.
  • Suitable compounds are derived, for example, from the substance classes of 4,4'-diamino-2,2'-stilbenedisulfonic acids (flavonic acids), 4,4'-distyrylbiphenyls, methylumbelliferones, coumarins, dihydroquinolinones, 1,3-diarylpyrazolines, naphthalic acid imides, benzoxazole, benzisoxazole and benzimidazole systems and the heterocyclic substituted pyrene derivatives.
  • fluor acids 4,4'-diamino-2,2'-stilbenedisulfonic acids
  • 4,4'-distyrylbiphenyls 4,4'-distyrylbiphenyls, methylumbelliferones, coumarins, dihydroquinolinones, 1,3-diarylpyrazolines, naphthalic acid imides, benzoxazole, benzisoxazole and benzimid
  • Preferred phosphonates are hydroxyalkane and aminoalkanephosphonates.
  • HEDP 1-hydroxyethane-1,1-diphosphonate
  • It is preferably used as the sodium salt, the disodium salt neutral and the tetrasodium salt alkaline (pH 9).
  • Preferred aminoalkane phosphonates are ethylenediamine tetramethylene phosphonate (EDTMP), diethylene triamine pentamethylene phosphonate (DTPMP) and their higher homologs. They are preferably in the form of neutral sodium salts, eg. B. as the hexasodium salt of EDTMP or as hepta- and octa-sodium salt of DTPMP used.
  • Bleach activators are used in detergents and cleaners and in the instant process of the present invention as the active ingredient in the active-product formulation to provide improved bleaching performance upon cleaning at temperatures of 60 ° C and below.
  • As bleach activators it is possible to use compounds which, under perhydrolysis conditions, give aliphatic peroxycarboxylic acids having preferably 1 to 10 C atoms, in particular 2 to 4 C atoms, and / or optionally substituted perbenzoic acid.
  • Suitable substances are those which carry O- and / or N-acyl groups of the stated C atom number and / or optionally substituted benzoyl groups.
  • polymeric polycarboxylates for example the alkali metal salts of polyacrylic acid or polymethacrylic acid, for example those having a relative molecular weight of 500 to 70,000 g / mol.
  • the molecular weights stated for polymeric polycarboxylates are weight-average molar masses M w of the particular acid form, which were determined in principle by means of gel permeation chromatography (GPC), a UV detector being used. The measurement was carried out against an external polyacrylic acid standard, which provides realistic molecular weight values due to its structural relationship with the polymers investigated. These data differ significantly from the molecular weight data, in which polystyrene sulfonic acids are used as standard. The molar masses measured against polystyrenesulfonic acids are generally significantly higher than the molecular weights specified in this document.
  • Suitable polymers are, in particular, polyacrylates which preferably have a molecular weight of 2,000 to 20,000 g / mol. Because of their superior solubility, the short-chain polyacrylates, which have molar masses of from 2000 to 10000 g / mol, and particularly preferably from 3000 to 5000 g / mol, may again be preferred from this group.
  • copolymeric polycarboxylates in particular those of acrylic acid with methacrylic acid and of acrylic acid or methacrylic acid with maleic acid.
  • Copolymers of acrylic acid with maleic acid which contain 50 to 90% by weight of acrylic acid and 50 to 10% by weight of maleic acid have proven to be particularly suitable.
  • Their relative molecular weight, based on free acids is generally from 2000 to 70000 g / mol, preferably from 20,000 to 50,000 g / mol and in particular from 30,000 to 40,000 g / mol.
  • biodegradable polymers of more than two different monomer units for example those which contain as monomers salts of acrylic acid and maleic acid and vinyl alcohol or vinyl alcohol derivatives or as monomers salts of acrylic acid and 2-alkylallylsulfonic acid and sugar derivatives ,
  • Suitable foam inhibitors include soaps, oils, fats, paraffins or silicone oils.
  • preferred active ingredient preparations contain paraffins, preferably unbranched paraffins (n-paraffins) and / or silicones, preferably linear polymeric silicones, which are constructed according to the scheme (R 2 SiO) x and are also referred to as silicone oils.
  • These silicone oils usually are clear, colorless, neutral, odorless, hydrophobic liquids having a molecular weight between 1,000 and 150,000, and viscosities between 10 and 1,000,000 mPa ⁇ s.
  • the active substance preparation preferably contains polymer and / or phosphonate, in particular in an amount of 0.5% to 15% by weight in each case. , based on the active ingredient preparation.
  • An advantage of the method according to the invention is that it makes possible the production of particulate detergent and cleaner compounds which, compared to carrier-free compounds (carrier materials according to the definition of the present invention) have a higher active ingredient content with comparable physical properties or the same Active substance content show improved physical properties.
  • the production according to the invention in a fluidized-bed granulator also makes it possible to further improve the physical properties of the granules, in particular their solubility and flowability.
  • the resistance to bleeding of the particulate detergent or cleaning agent compounds produced by the process according to the invention is improved in comparison to formulations of the same formulation prepared in mixers with mixing tools and tumble mixers.
  • Another object of the present invention is a detergent or cleaning agent compound, which is composed of a core and at least two shells and a support material from the group of amorphous aluminosilicates, clays, silicas, alkaline earth metal silicates, alkaline earth metal carbonates, and at least 30 wt .-% of one or more Active ingredient (s) from the list of nonionic surfactants, anionic surfactants, cationic surfactants, optical brighteners, phosphonates, bleach activators, polymers and foam inhibitors.
  • the detergent or cleaning agentcomposition according to the invention preferably prepared by the process according to the invention, preferably contains at least 40% by weight, more preferably at least 50% by weight, more preferably at least 60% by weight, with particular preference at least 70% by weight. , more preferably at least 80 wt .-%, preferably at least 90 wt .-% and in particular at least 95 wt .-% of one or more active ingredients, in particular from the group of nonionic surfactants, anionic surfactants, cationic surfactants, optical brighteners, phosphonates, bleach activators , Polymers and foam inhibitors.
  • the detergent or cleaning agent compound are at 2 to 30 wt .-%, preferably at 2 to 25 wt .-%, particularly preferably 2 to 20 wt .-% and in particular at 3, 4, 5, 6, 7 or 8 bis 10, 11, 12, 13, 14 or 15 wt .-% of a support material or a plurality of support materials from the group of amorphous aluminosilicates, clays, silicas, alkaline earth metal silicates, alkaline earth metal carbonates.
  • the detergent or cleaning agent compound according to the invention preferably prepared by the process according to the invention, advantageously has a bulk density in the range from 450 to 850 g / l, preferably from 500 to 800 g / l, particularly preferably from 550 to 750 g / l and in particular from 600 to 750 g / l on.
  • particulate when using a solvent or dispersant-containing active ingredient preparation in the process according to the invention particulate, to be designated as flowable detergent or cleaning agent compounds having an active ingredient content above 50 wt .-%, based on the amount of active in the wash or detergent compound, while a process which differs only in the choice of granulator (high shear mixer) from the process according to the invention, does not provide a particulate product, but a product pulp with large lumps of insufficiently mixed components.
  • a part of the carrier material preferably 10-90% by weight of the carrier material used in the process, is mixed with the liquid to pasty active substance preparation to form a pumpable and / or extrudable mass, before this mass is fed into the fluidized bed granulator.
  • This procedure is particularly advantageous when the active substance preparation used in the process less than 20 wt .-%, preferably less than 10 wt .-%, preferably less than 5 wt .-% and in particular less than 2.5 wt .-% solution - Or dispersant, based on the active ingredient preparation contains.
  • the support material used in the process according to the invention may be advantageous to use a large part of the support material used in the process according to the invention, for example up to 90% by weight, preferably from 20 to 85% by weight, particularly preferably from 30 to 80% by weight, to this end preferably 40 to 75 wt .-%, preferably 50 to 70 wt .-% and in particular 60 to 65 wt .-% of the carrier material with the active compound preparation to a pumpable and / or extrudable mass before mixing this mass in the fluidized bed Granulator is fed.
  • at least part of the support material used in the process is fed as a solid into the fluidized bed granulator.
  • products of the process according to the invention have improved physical properties compared to products of a granulation process in a fluidized bed granulator in which carrier materials were fed exclusively via a pumpable and / or extrudable mass, but not as a solid in the fluidized bed granulator , in particular have an improved flowability with exceptionally high active ingredient content and a reduced tendency to bleed.
  • the active ingredient formulation contains at least 20% by weight, preferably at least 25% by weight, more preferably at least 30% by weight, more preferably at least 35% by weight, more preferably at least 40% by weight, more preferably at least 45% by weight, preferably at least 50% by weight and in particular at least 55% by weight of solvent or dispersant
  • less than 60% by weight, preferably less than 50% by weight is preferred less than 40% by weight, more preferably less than 30% by weight, even more preferably less than 20% by weight, with preference less than 10% by weight and in particular less than 5% by weight of the Method used carrier material with the active ingredient preparation are mixed into a mass before this mass is fed into the fluidized bed granulator.
  • the process according to the invention is preferably carried out at fluidization rates of between 1 and 8 m / s and in particular between 1.2 and 5.5 m / s.
  • Granules preferred according to the invention have a d 50 value between 0.1 and 2.5 mm.
  • the grain fraction which is greater than 1.6 mm, is recycled. This coarse grain fraction can either be added to the fluidized bed granulator as a solid component after grinding or it is dissolved and mixed with the active substance preparation and recycled together with this in the fluidized bed.
  • the d 50 value of the product obtained from the fluidized bed granulator in the range of 0.1 to 0.8 mm, in particular from 0.2 to 0.6 mm, when the detergent or cleaning compound with other particulate components to a End product to be mixed, which has an average particle size d 50 in this area.
  • the detergent or cleaning agent compound is to be mixed into a coarser detergent or cleaning agent, it may be preferable to adjust the separator air flow so that the product from the fluidized bed granulator has a mean particle size d 50 in the range from 0.7 to 1.6 mm, in particular in the range of 0.9 to 1.4 mm.
  • the carrier material or the part of the carrier material which is fed into the fluidized-bed granulator as a solid is preferably introduced by means of Duckluft, preferably at 10 - 50 m / s, in particular at 20 - 40 m / s in the granulation space.
  • the or the entry point of the solid can be positioned directly above the distributor plate of the fluidized bed granulator, in the region between the distributor plate and the upper limit of the fluidized bed formed by the fluidization of the particles contained in the fluidized bed granulator or even above the upper limit of the fluidized bed be.
  • the height or (upper) limit of the fluidized bed is here the position in the fluidizing granulator, between which and the distributor plate are at least 90 wt .-% of the particles contained in the fluidization granulator at the time considered.
  • the carrier material used in the process preferably at least 30 wt .-%, preferably at least 45 wt .-%, more preferably at least 60 wt .-% and in particular at least 75 wt .-% of the solid in the process used carrier material in the fluidized bed granulator in the lower three quarters, preferably in the lower half and in particular in the lower third of the height of the formed in the fluidized bed granulator fluidized bed, the carrier material used in the process according to the invention to a much smaller part by the fluidizing air discharged from the fluidized bed than in conventional processes in which fine particles are fed to the fluidization space at a higher point of the fluidized-bed granulator seen from the distributor bottom.
  • the feed points for the carrier material are preferably positioned no further than 50 cm, preferably not more than 30 cm and in particular not more than 10 cm away from the distributor plate in the direction of the upper limit of the fluidized bed.
  • fine particles are those which have an average particle size d 50 below 200 ⁇ m, in particular below 100 ⁇ m.
  • the term "average particle diameter d 50" is understood to mean the value at which 50% of the particles have a smaller diameter and 50% of the particles (in each case based on the particle mass) have a larger diameter.
  • the fluidization space here is located above the inflow floor in a fluidized bed granulator space, which is not distinguished between Fluidleitersraum and sedation and the term Fluidmaschinesraum instead also includes the area of the sedative space.
  • the carrier material can be fed, for example, tangentially or radially into the fluidized bed.
  • the feed of the carrier material takes place at an angle of 30 to 90 ° C in the fluidized bed, wherein the angle of attack is measured so that an angle of 90 ° corresponds to a tangential and 0 ° a radial position and thus the angle between the feed direction and the "extended radius line" of the round fluidized bed is determined.
  • the angle of attack of the carrier material feed is 45-70 ° and in particular 50-60 °.
  • the feed points for the carrier material are preferably positioned on the wall surfaces of the fluidization space and are not in the immediate vicinity of the corners, in which two wall surfaces collide.
  • the feed points are at least 1/20 of the horizontal area width, preferably at least 1/10 and in particular at least 1/5 of the horizontal area width of each adjacent to the corner surface on which the feed point is located away from the corners.
  • the feed of the carrier material is preferably carried out in the direction of the center of the fluidization space.
  • the carrier material at an angle of 0 to 80 ° in the fluidized bed, this angle between Einspeiseraum and orthogonal to the wall surface on which the feed point is determined.
  • the feed in the direction of the orthogonal corresponds to an angle of 0 ° and a feed along the wall surface at an angle of 90 °.
  • the carrier material is preferably fed horizontally or in the direction of the inflow bottom, ie downwards, into the fluidized bed.
  • the feed direction with the horizontal preferably includes an angle in the range from 1 to 80 °, preferably 3 to 75 °, particularly preferably 5 to 70 ° and in particular 7 to 65 °.
  • the advantage of this measure is a further increase in the residence time of the fine carrier material in the fluidized bed.
  • the average particle size of the support material in a pre-stored granulation of Aktivstoffzurung process step to 25 to 100 .mu.m, preferably 35 to 100 .mu.m, more preferably 45 to 100 .mu.m and in particular 55 to 100 microns preset.
  • This process step which precedes the granulation of the active substance preparation, is preferably carried out in a mixer with mixing tools or in a free-fall mixer.
  • the spray-drying of a carrier slurries which In addition to the carrier material and a liquid component optionally further components, such as structural means contains, is conceivable.
  • the carrier material is preferably mixed with structuring agents and granulated.
  • An advantage of adjusting the particle size of the carrier material to the specified range is the reduced dust tendency of the carrier material when carrying out the method according to the invention. As a result, less contamination of the environment and the process carrying staff with the fine carrier material occurs and the carrier material remains due to the higher weight of the precursor prepared carrier granules in the lower part of the fluidized bed and becomes a much smaller part by the fluidizing gas from the fluidized bed discharged and deposited in the filters.
  • the structuring agents used are preferably water-soluble constituents of detergents or cleaners and in particular water-soluble polymers.
  • the use of polycarboxylates as structurant is particularly preferred.
  • the preferably used water-soluble structuring agents dissolve rapidly in the aqueous washing or cleaning liquor, so that the formed “coarse” carrier material particles disintegrate in the washing or cleaning liquor and thus not as “coarse”, water-insoluble residues on the cleaned surface, especially the washed laundry remain.
  • Both the feeding of the carrier material or a part of the carrier material in the vicinity of the inflow base, as well as the selected feed angle of the carrier material, as well as the previously described prior particle size adjustment of the carrier material result in that the commercially available and commonly used form can be characterized as being fine Carrier material longer in the fluidized bed remains, as is the case when the carrier material is fed into a fluidized bed granulator in a well-known manner. As a result, there is a reduced discharge of the support material from the fluidized bed and less carrier material is deposited in the internal or external filters of the fluidized bed granulator.
  • the active substance preparation is preferably sprayed onto the moving carrier material by means of two-component spray nozzles.
  • the active substance preparation is preferably sprayed as evenly as possible on the carrier material and the optional further component (s). If the active substance preparation can not be sprayed, it is preferably pumped or extruded into the Fluidized bed granulator fed. In addition, it is possible and particularly preferred to feed the active substance preparation in the form of a foam into the fluidized-bed granulator.
  • the product of the process according to the invention can be used as a particulate detergent or cleaning agent compound and mixed with further particulate components of a washing or cleaning agent. Alone or after mixing with other particulate components, the detergent or cleaning agent compound according to the invention can be extruded, pressed or dispersed in liquid to gelatinous preparations.
  • Another object of the present invention is a washing or cleaning agent in granular, liquid to gel or compressed form comprising 1 to 99 wt .-% of a detergent or cleaning agent compound prepared by the process according to the invention.
  • an additional process step to the granulation step of the process according to the invention and, after granulation of the active substance preparation on the particles obtained, a liquid component, preferably selected from the group of nonionic and cationic surfactants, perfume oils, foam inhibitors, optical brighteners and phosphonates is going to raise.
  • This additional process step can be carried out in all mixers known to the person skilled in the art, preferably in one of the above-mentioned mixers or in mixer combinations.
  • the granulate resulting from this optional additional process step advantageously has a bulk density in the range from 450 to 1000 g / l, preferably from 500 to 900 g / l, particularly preferably from 550 to 850 g / l and in particular from 600 to 800 g / l ,
  • the d 50 value is preferably in the range of 0.1 to 0.8 mm, in particular 0.2 to 0.6 mm, when the granules are to be used as detergent and Renistsffencompound that with other particulate components to a End product to be mixed, which has an average particle size d 50 in this area.
  • the mean particle size d 50 is preferably in the range from 0.7 to 1.6 mm, in particular in the range from 0.9 to 1.4 mm .
  • the particulate product formed after this additional step downstream of the granulation can in turn be used as a particulate detergent or cleaning compound and mixed with further particulate components of a washing or cleaning agent, extruded alone or after mixing with further particulate components, compressed or in liquid to gelatinous formulations be dispersed.
  • the other particulate components with which the detergent or cleaning agent compound is mixed to provide a solid detergent or cleaning agent may be any of the granules, powders, extrudates, agglomerates or moldings known to those skilled in the art.
  • Preferred ingredients of the other particulate components are preferably selected from the group of builders, surfactants, polymers, bleaches, bleach activators, bleach catalysts, enzymes, disintegrants, fragrances, perfume carriers, electrolytes, pH adjusters, fluorescers, hydrotopes, foam inhibitors, silicone oils, anti redeposition agents, optical brighteners , Graying inhibitors, anti-shrinkage agents, anti-crease agents, color transfer inhibitors, antimicrobial agents, germicides, fungicides, antioxidants, antistatic agents, ironing aids, repellents and impregnating agents, swelling and anti-slip agents and UV absorbers selected.
  • liquid or pasty detergent or cleaning agent components can be sprayed onto the mixture of the detergent or cleaning agent compound and the one or more
  • disintegration aids so-called tablet disintegrants
  • tablet disintegrants or disintegrants are meant excipients which ensure the rapid disintegration of tablets in water or other media and for the rapid release of the active ingredients.
  • the particulate detergent or cleaning compound is introduced into a liquid or gel detergent or cleaning agent, it preferably contains a thickener.
  • the thickener may include, for example, a polyacrylate thickener, xanthan gum, gellan gum, guar gum, alginate, carrageenan, carboxymethyl cellulose, bentonites, wellan gum, locust bean gum, agar, tragacanth, gum arabic, pectins, polyoses, (modified) starch, dextrins, Include gelatin and casein.
  • the viscosity of the liquid detergents and cleaners can be measured by standard methods and is preferably in the range from 500 to 5000 mPas (measured with a Brookfield LVT-II at 20 rpm and 20 ° C., spindle 3).
  • Preferred agents have viscosities from 700 to 4000 mPas, with values between 1000 and 3000 mPas being particularly preferred.
  • liquid detergents and cleaners are prepared by customary and known methods and processes in which, for example, the constituents are simply mixed in stirred kettles, whereby water, non-aqueous solvents and surfactant (s) are advantageously introduced and the further constituents are added in portions. Separate heating in the preparation is not required, if desired, the temperature of the mixture should not exceed 80 ° C.
  • the particulate detergent or cleaning compound compound can be stably dispersed in the liquid detergent and cleaning agent, for example, by stirring.
  • Stable means that the compositions are stable at room temperature and at 40 ° C for a period of at least 4 weeks and preferably at least 6 weeks, without the detergent or cleaning agent granules being creamed or sedimented.
  • the detergent or cleaning agent granules are provided with a coating prior to introduction into the liquid or gel agent.
  • coating materials it is possible to use polymers which do not dissolve in the matrix with a relatively low water concentration.
  • the detergent or cleaning agent compound or a washing or cleaning agent comprising at least 1 wt .-% of the detergent or cleaning agent tablets, such as ring or pill tablets, which may have several compressed and optionally not compressed phases obtained. It is also possible to fill the washing or cleaning agent in a sachet, for example a pouch, whose casing is preferably formed from at least partially translucent, water-soluble or water-dispersible film.
  • the sachet can also have several chambers and in addition to the detergent or cleaning agent in granular or compressed form further granular, compressed, liquid and / or gelatinous components.
  • Aim Preparation of granular detergent or cleaner compounds comprising about 60% by weight of anionic surfactant, about 4% by weight of silica and about 36% by weight of zeolite A (including water)
  • an aqueous alkylbenzenesulfonate paste is used (Maranil A 55, manufacturer Cognis).
  • the paste contains 55% by weight of alkylbenzenesulfonate, about 2% by weight of salts / other and about 33% by weight of water and is heated to 60 ° C. before use.
  • Zeolite A manufactured Zeoline SA, water content about 19 - 21 wt .-%) Silica (Sipernat 22S, manufacturer Degussa) Both solids have an average particle size d 50 below 10 microns.
  • Example 1 (according to the invention):
  • a fluidized-bed granulator (Glatt, type AGT 400) 15 kg of granules are submitted from a previous process run as a starting material and made with 1000 m 3 / h at a supply air temperature of 160 ° C for whirling.
  • the active substance preparation is continuously fed via a central two-component nozzle with a mass flow of 10.9 kg / h, and the silica and zeolite A via a rotary valve with a mass flow of 400 g / h (silicic acid) or 3.6 kg / h (zeolite A) fed into the fluidized bed granulator.
  • the process runs continuously over several hours.
  • L test To determine the solubility behavior (L test), 8 g of the granules to be tested are sprinkled in a 2 l beaker with stirring (800 rpm with laboratory stirrer / propeller stirring head centered 1.5 cm from the beaker bottom) and 1.5 minutes stirred at 30 ° C. The test is carried out with water of a hardness of 16 ° d. The caustic is then poured off through a sieve (80 ⁇ m). The beaker is rinsed with very little cold water over the sieve. There is a 2-fold determination. The sieves are dried in a drying oven at 40 ° C ⁇ 2 ° C to constant weight and the residue is weighed out.
  • the material obtained is then transferred to a rectangular fluidized bed apparatus (Heinen, WT 5/30 L-S) for drying.
  • a supply air speed of 0.6 m / s supply air temperature 120 ° C
  • the conidor bottom immediately occupies the inlet.
  • the lumps can not get through the fluidized bed to the exit and dry at the same time. The attempt is canceled.
  • a fluidized bed granulator (Glatt, type AGT 1800) 1700 kg granules are submitted from a previous process run as a starting material and made to vortex at 18000 m 3 / h at a supply air temperature of 150 ° C.
  • the active substance preparation (as in Example 1) is continuously fed via three two-component nozzles with a mass flow of 750 kg / h, and the silica (as in Example 1) and the zeolite A (as in Example 1) via pneumatic lines with a mass flow of 50 kg / h (silica) or 252 kg / h (zeolite A) fed into the fluidized bed granulator.
  • Silica (Sipernat 22S, manufacturer Degussa, average particle size d 50 ⁇ 10 ⁇ m)
  • Spray-dried zeolite-based powder (about 75% by weight of zeolite A, bulk density 450 g / l, average particle size d 50 about 0.45 mm)
  • a fluidized bed granulator (smooth, type AGT 400, Zu Kunststofftempertur 25 ° C, supply air 810 m 3 / h) are continuously the active ingredient preparation via a two-fluid nozzle with a mass flow of 12 kg / h, and the silica and the spray-dried powder via a rotary valve with a mass flow of 1.2 kg / h (silica) or 9.6 kg / h (spray-dried powder) fed.
  • the resulting granules are flowable, contain 52 wt .-% of nonionic surfactant and have an average particle size d 50 of 0.55 mm a bulk density of 642 g / l.

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  • Life Sciences & Earth Sciences (AREA)
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Claims (9)

  1. Procédé pour la production d'un composite particulaire d'agent de lavage ou de nettoyage par granulation d'une préparation de substance active liquide à pâteuse à une température de 0 à 100 °C, via l'addition par mélange d'une substance solide dans un dispositif de granulation en lit fluidisé, caractérisé en ce que la substance solide contient une ou plusieurs matières de support choisies parmi le groupe des aluminosilicates amorphes, des argiles, des acides siliciques, des silicates de métaux alcalino-terreux, des carbonates de métaux alcalino-terreux, la granulométrie moyenne d50 de la matière de support est inférieure à 100 µm et le composite d'agent de lavage ou de nettoyage contient de 2 à 30 % en poids d'une ou plusieurs des matières de support.
  2. Procédé selon la revendication 1, caractérisé en ce que la préparation de substance active contient au moins une substance active et un solvant ou un agent de mise en dispersion, et en ce que, au cours de la granulation, on élimine au moins en partie le solvant ou l'agent de mise en dispersion.
  3. Procédé selon l'une quelconque des revendications 1 ou 2, caractérisé en ce que la préparation de substance active contient une ou plusieurs substances actives choisies parmi la liste des agents tensioactifs non ioniques, des agents tensioactifs anioniques, des agents tensioactifs cationiques, des azurants optiques, des phosphonates, des activateurs du blanchiment, des polymères et des inhibiteurs de mousse.
  4. Procédé selon l'une quelconque des revendications 2 ou 3, caractérisé en ce qu'on introduit au moins une partie de la matière de support dans le dispositif de granulation en lit fluidisé, dans les trois quarts inférieurs, de préférence dans la moitié inférieure et en particulier dans le tiers inférieur de la hauteur du lit fluidisé mis en oeuvre dans le dispositif de granulation en lit fluidisé.
  5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce qu'on mélange une partie de la matière de support, de préférence de 10 à 90 % en poids de la matière de support mise en oeuvre dans le procédé, avec la préparation de substance active liquide à pâteuse afin d'obtenir une masse apte à être pompée et/ou apte à être extrudée, avant d'introduire cette masse dans le dispositif de granulation en lit fluidisé.
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce qu'après la granulation, sur les particules obtenues, on applique un composant liquide, de préférence choisi parmi le groupe des agents tensioactifs non ioniques et cationiques, des essences de parfum, des inhibiteurs de mousse, des azurants optiques, des phosphonates.
  7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce qu'après la granulation et l'application facultative d'un composant liquide sur les particules obtenues, on extrude les produits de granulation résultants, à titre individuel ou après mélange avec d'autres composants de forme particulaire, on les comprime ou on les disperse dans des préparations liquides à géliformes.
  8. Composite d'agent de lavage ou de nettoyage, qui se compose d'un noyau et d'au moins deux enveloppes et qui comprend une matière de support choisie parmi le groupe des aluminosilicates amorphes, des argiles, des acides siliciques, des silicates de métaux alcalino-terreux, des carbonates de métaux alcalino-terreux, ainsi qu'au moins 30 % en poids d'une ou de plusieurs substances actives choisies parmi la liste des agents tensioactifs non ioniques, des agents tensioactifs anioniques, des agents tensioactifs cationiques, des azurants optiques, des phosphonates, des activateurs du blanchiment, des polymères et des inhibiteurs de mousse, et que l'on prépare conformément à un procédé selon l'une quelconque des revendications 1 à 7.
  9. Agent de lavage ou de nettoyage sous forme granuleuse, liquide à géliforme ou comprimée comprenant de 1 à 99 % en poids d'un composite d'agent de lavage ou de nettoyage que l'on prépare conformément à un procédé selon l'une quelconque des revendications 1 à 7.
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HUE026232T2 (en) * 2011-09-30 2016-06-28 Unilever Nv Method and composition for cleaning hard surfaces
CN103998592A (zh) * 2011-09-30 2014-08-20 荷兰联合利华有限公司 清洁硬表面的方法和组合物
DE102016223472A1 (de) 2016-11-25 2018-05-30 Henkel Ag & Co. Kgaa Mehrkammer-Portionsbeutel mit Bleichaktivator/Komplexbildner-Compound

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US6858572B1 (en) * 1999-03-09 2005-02-22 The Procter & Gamble Company Process for producing coated detergent particles
DE50011442D1 (de) * 2000-02-18 2005-12-01 Glatt Ingtech Gmbh Verfahren zur Herstellung von Vollwaschmitteln und Vollwaschmittelkomponenten
GB0125653D0 (en) * 2001-10-25 2001-12-19 Unilever Plc Process for the production of detergent granules

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Title
ANONYMOUS: "Kontinuierliche Technologien", 30 April 2006 (2006-04-30), XP055032243, Retrieved from the Internet <URL:http://www.glatt.com/cm/fileadmin/material/equipment/pdfs/continuous_technologies_d.pdf> [retrieved on 20120710] *

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EP2207871A2 (fr) 2010-07-21
PL2207871T3 (pl) 2014-05-30

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