WO2024022962A1 - Composition de détergent textile - Google Patents

Composition de détergent textile Download PDF

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Publication number
WO2024022962A1
WO2024022962A1 PCT/EP2023/070249 EP2023070249W WO2024022962A1 WO 2024022962 A1 WO2024022962 A1 WO 2024022962A1 EP 2023070249 W EP2023070249 W EP 2023070249W WO 2024022962 A1 WO2024022962 A1 WO 2024022962A1
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WO
WIPO (PCT)
Prior art keywords
agent
active ingredient
granule
layering
composition according
Prior art date
Application number
PCT/EP2023/070249
Other languages
English (en)
Inventor
Panchanan BHUNIA
Sujitkumar Suresh Hibare
Hemendra Dilip JOSHI
Shashank Khare
Rajan Chandrakant MHAMUNKAR
Original Assignee
Unilever Ip Holdings B.V.
Unilever Global Ip Limited
Conopco, Inc., D/B/A Unilever
Priority date (The priority date 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 date listed.)
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Publication date
Application filed by Unilever Ip Holdings B.V., Unilever Global Ip Limited, Conopco, Inc., D/B/A Unilever filed Critical Unilever Ip Holdings B.V.
Publication of WO2024022962A1 publication Critical patent/WO2024022962A1/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
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66—Non-ionic compounds
    • C11D1/72—Ethers of polyoxyalkylene glycols
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/88—Ampholytes; Electroneutral compounds
    • C11D1/90—Betaines
    • 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
    • C11D17/0034—Fixed on a solid conventional detergent ingredient
    • 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
    • C11D3/046—Salts
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/10—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
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • 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
    • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
    • 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
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/2075—Carboxylic acids-salts thereof
    • C11D3/2086—Hydroxy carboxylic acids-salts thereof
    • 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
    • C11D3/26—Organic compounds containing nitrogen
    • C11D3/33—Amino carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/36—Organic compounds containing phosphorus
    • C11D3/361—Phosphonates, phosphinates or phosphonites
    • 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
    • C11D3/36—Organic compounds containing phosphorus
    • C11D3/364—Organic compounds containing phosphorus containing nitrogen

Definitions

  • laundry detergent composition contains a base powder, prepared by spray-drying or granulation or a combination of such processes.
  • Base powder consists of structured particles containing all, or a major part of, the surfactant and builder in the formulation.
  • Other ingredients not suitable for incorporation in the base powder such as bleaches, enzymes, heat-sensitive co-surfactants, antiredeposition polymers, dye transfer inhibiting polymers, foam control agent, sequestrant and perfumes are subsequently sprayed on to, or dry mixed with, the base powder.
  • Some of these post dosed ingredients in particulate form are hygroscopic and may absorb a significant amount of water from the atmosphere thus leading to caking of said particles during manufacturing, packing, storage and/or dosing by the user.
  • To keep the solid laundry detergent composition free flowing it is necessary that the other ingredients that are post dosed into the base power do not influence the powder properties of the detergent composition.
  • several ways for solving the problem of incorporating hygroscopic ingredient or a liquid active ingredient into particulate solid compositions have been proposed.
  • a powder or granulate active ingredient mainly consisting of the hygroscopic ingredient
  • a non-hygroscopic ingredient may be coated with a non-hygroscopic ingredient, thus impeding the uptake of water by the (now coated) hygroscopic active ingredient.
  • This approach solves the problem associated with hygroscopicity; however, coating is an expensive process, and thus production costs significantly rise.
  • incorporating a liquid active ingredient into a base powder it may either be sprayed onto or mixed with the base powder.
  • the inventors of the present invention have surprisingly found that when the active ingredient is incorporated in a co-granule, where the co-granule has the active ingredient in combination with a layering agent and a hydrating agent and where the blend of layering agent and a hydrating agent is incorporated in specific weight ratios between the layering agent and the hydrating agent it provides for a free-flowing, solid co-granule which has extended shelf life and good anticaking properties.
  • the co-granule can be used in combination with other laundry adjuvants to prepare the final solid laundry detergent formulations to provide improved powder properties.
  • a solid laundry detergent composition comprising a co-granule, the co-granule comprising: (i) an active ingredient wherein the active ingredient is either a solid having a moisture content ranging from 0 wt.% to 20 wt.% or the active ingredient is a liquid having a viscosity less than 1000 millipascal second; (ii) a layering agent; (iii) a hydrating agent; wherein the active ingredient is intimately mixed with the hydrating agent and the layering agent and wherein weight ratio of the amount of the layering agent to the hydrating agent ranges from 1:2.5 to 1:19 in the co-granule and wherein the co-granule comprises less than 10 wt.% anionic surfactant.
  • a process for preparing the co-granule of the first aspect includes the steps of: (i) obtaining a hydrating agent, a layering agent and an active ingredient wherein the active ingredient is either a solid having a moisture content ranging from 0 wt.% to 20 wt.% or a liquid having a viscosity less than 1000 millipascal second; (ii) homogeneously mixing the hydrating agent and the active ingredient to form a mixture; (iii) adding the layering agent to the mixture obtained in step (ii) to form a co-granule; wherein the weight ratio of the amount of the layering agent to the hydrating agent ranges from 1:2.5 to 1:19 in the co-granule and wherein the co-granule comprises less than 10 wt.% anionic surfactant.
  • co-granule means a granule including more than one compound or component.
  • granule means various solid forms which includes but is not limited to powders, granulate, coarse powder, tablets, needles, and noodles.
  • hygroscopic ingredient means a (i) liquid material which upon exposure to hot and humid air (30°C to 40°C and relative humidity of 80 to 85% RH) becomes less concentrated or form viscous gel phases or (ii) a solid material which upon exposure to hot and humid air (30°C to 40°C and relative humidity of 80 to 85% RH) becomes fluid or forms agglomerates/cakes.
  • the hygroscopicity is measured by storing a sample until equilibrium in a climate box at 28° C. and 60% relative humidity and recording the weight increase as a percentage of the starting weight (wt %).
  • the tendency to form agglomerates is tested visually by establishing whether the sample is free flowing or not or is measured in a so-called caking test cylinder and is expressed as a caking value.
  • a low caking value is desirable for prolonged storage of the active ingredient. It is preferred that the Compressibility (caking value) is less than 2000 grams, and the volume compression testing (VCT) is less than 30%.
  • the hygroscopic active ingredient used in the present invention has a hygroscopicity value above 1 wt.%, preferably above 2 wt.%, more preferably above 4 wt.%, most preferably above 8 wt %.
  • the non-hygroscopic co-granule of the invention has a hygroscopicity lower than 8 wt.%, preferably lower than 4 wt.%, more preferably lower than 3 wt.%, most preferably lower than 2 wt %.
  • the caking value of the co-granule according to the invention is lower than 10, preferably lower than 5, most preferably lower than 3.
  • the water content of the co-granule is lower than 8 wt.%, preferably lower than 4 wt.%, most preferably lower than 2 wt %.
  • a solid laundry detergent composition comprising a co-granule.
  • Co-granule includes an active ingredient, a layering agent, and a hydrating agent.
  • the co-granule according to the present invention preferably has a glass transition temperature of more than 45°C. The glass transition temperature is measured using the method Differential Scanning Calorimetry (DSC).
  • the co-granule has a weight average particle size ranging from 180 to 1000 micrometers. More preferably the co-granule has a weight average particle size ranging from 300 to 1000 micrometers. Preferably the co-granule according to the present invention has a weight average particle size ranging from 200 to 800 micrometers, still preferably from 300 micrometers to 700 micrometers.
  • the co-granule has a weight average particle size which is at least 185 micrometers, preferably at least 190 micrometers, still preferably at least 195 micrometers, still more preferably at least 200 micrometers and most preferably at least 300 micrometers, but typically not more than 950 micrometers, still preferably not more than 900 micrometers, still further preferably not more than 850 micrometers, further preferably not more than 700 micrometers and most preferably not more than 500 micrometers.
  • the co-granule is a free-flowing particle and has a dynamic flow rate of 60 mL/s to 120 mL/s when measured using a DFR apparatus-502A from Silikon Technologies.
  • the co-granule according to the present invention includes less than 10 wt.% anionic surfactant. Still preferably the co-granule according to the present invention includes less than 8 wt.% anionic surfactant, still preferably less than 5 wt.% anionic surfactant, still more preferably less than 3 wt.% anionic surfactant and more preferably 0 wt.% anionic surfactant.
  • anionic surfactant consists of the group selected from sulphonate anionic surfactant, sulphate anionic surfactant, soap and mixtures thereof.
  • anionic surfactant is meant those selected from the group consisting of sulphonate anionic surfactant, non-alkoxylated sulphate anionic surfactant, soap and mixtures thereof.
  • the amount of the sulphonate anionic surfactant, non-alkoxylated sulphate anionic surfactant, soap and mixtures thereof either alone or combination is less than 10 wt.%, still preferably less than 8 wt.%, still preferably less than 5 wt.%, still more preferably less than 3 wt.% and most preferably less than 0 wt.%.
  • the co-granule includes from 5 wt.% to 50 wt.% of the active ingredient.
  • the amount of the active ingredient in the co-granule is not less than 8 wt.%, still preferably not less than 10 wt.%, more preferably not less than 15 wt.% still more preferably not less than 20 wt.%, but it is preferred that the amount of the active ingredient in the co-granule is not more than 50 wt.%, still more preferably not more than 40 wt.%, still more preferably not more than 35 wt.%, furthermore preferably not more than 25 wt.%.
  • Active ingredient According to the first aspect of the present invention the co-granule includes an active ingredient.
  • the active ingredient may be either a solid or a liquid.
  • the active ingredient When the active ingredient is a solid it has a moisture content ranging from 0 wt.% to 20 wt.% by weight of the active ingredient.
  • the solid active ingredient has a moisture content of at least 1 wt.%, preferably at least 2 wt.%, still preferably at least 3 wt.% and most preferably at least 5 wt.%, but typically not more than 15 wt.%, still preferably not more than 13 wt.%, still further preferably not more than 11 wt.%, and most preferably not more than 10 wt.% by weight of the active ingredient.
  • the moisture content of the active ingredient is measured by taking a known weight of the active ingredient and spreading the active ingredient thinly on a petri plate, the weight of the petri plate (W1) and the weight of the petri plate along with the active ingredient (W2) was measured. Next the petri plate along with the active ingredient was dried using infrared light source or a halogen lamp at a temperature ranging from 130°C to 135°C till the completion of a predetermined drying time. At the end of the drying time, the weight of the petri plate is constant and this weight is recorded as (W3).
  • the solid active ingredient has a surface area ranging from 100 cm 2 /g to 350 cm 2 /g most preferably from 150 cm 2 /g to 300 cm 2 /g.
  • the surface area is measured using a particle size measuring device, CAMSIZER (model no.X2) from Retsch.
  • the surface area is determined using the mass-based specific surface area using the formula: where : Sm is the mass based surface are of the particle A is the surface area of the particle M is the mass of all the particles xi denotes the particle.
  • the active ingredient When the active ingredient is a liquid, it has a viscosity less than 1000 millipascal second, still preferably the viscosity is less than 900 millipascal second.
  • the viscosity of the liquid was measured using a Haake Viscometer at 30°C to 60°C at a shear rate of 20s -1 .
  • the active ingredient in the liquid form may be preferably an aqueous solution having a water content ranging from 35 wt.% to 80 wt.% by weight of the liquid active ingredient, still preferably having a water content ranging from 35 wt.% to 50 wt.% by weight of the liquid active ingredient.
  • the viscosity of the liquid active ingredient was measured using a Haake Viscometer apparatus.
  • the Haake viscometer applies a controlled stress to a liquid sample and measures the resulting deformation.
  • the sample is placed into a temperature controlled cylindrical cup, in which a rotor (or “bob”) rotates.
  • the rotor is rotated at a constant rate and the resulting torque measured by the machine is translated into a stress.
  • the viscosity is calculated from a ratio of the stress to the shear rate.
  • the Haake viscometer is provide with a microchip which is programmed to measure the parameters for viscosity calculation and the viscosity is digitally displayed.
  • the active ingredient is a hygroscopic ingredient which is used in a solid laundry composition.
  • the active ingredient is selected from the group consisting of but not limited to sequestrant, co-surfactant, polymer, or derivatives thereof, foam controlling agent, or a combination thereof. More preferably the active ingredient is selected from the group consisting of sequestrant, co-surfactant, polymer, or derivatives thereof, foam controlling agent, and mixtures thereof.
  • the active ingredient according to the present invention does not encompass anionic surfactant selected from the group consisting of anionic sulphonate surfactant, anionic alkyl sulphate surfactant, soap, and mixtures thereof.
  • the active ingredient includes 0 wt.% anionic surfactant selected from the group consisting of anionic sulphonate surfactant, anionic alkyl sulphate surfactant, soap, and mixtures thereof.
  • Sequestrant Preferably the active ingredient is a sequestrant. Still preferably the sequestrant is an aminopolycarboxylate compound.
  • the aminopolycarboxylate compound is selected from the group consisting of methylglycinediacetic acid (MGDA), ethylenediaminedisuccinic acid (EDDS), glutamic acid N, N-diacetic acid (GLDA), iminodisuccinic acid (IDS), trisodium nitrilotriacetate (NTA), iminodimalic acid (IDM) or mixtures thereof.
  • MGDA methylglycinediacetic acid
  • EDDS ethylenediaminedisuccinic acid
  • GLDA N-diacetic acid
  • IDDS iminodisuccinic acid
  • NDA trisodium nitrilotriacetate
  • IDM iminodimalic acid
  • the aminopolycarboxylate sequestrant is MGDA, GLDA, or mixtures thereof.
  • the sequestrant may preferably be an aliphatic polyhydroxy monocarboxylate.
  • These compounds are characterized by the presence therein of from 3 to 10 or more carbon atoms, at least two hydroxyl groups and most frequently one hydroxyl group attached to each carbon atom including the carboxyl carbon atom, and certain instances such as in the case of material derived from fructose, a carbonyl group intermediate the ends of the aliphatic chain.
  • these acids contain 5 or 6 carbon atoms and an equal number of hydroxyl groups including a hydroxyl group forming a part of the carboxyl group.
  • Suitable examples of aliphatic polyhydroxy monocarboxylate include but is not limited to alkali metal salts, alkaline earth metal salts, ammonium salt of gluconate, glucoheptanate, mannonate, glycerate or mixtures thereof. More preferably the aliphatic polyhydroxy monocarboxylate is an alkali metal salts gluconate, glucoheptanate, mannonate, glycerate or mixtures thereof. Preferably the alkali metal is selected from sodium, potassium, more preferably sodium. Most preferably the aliphatic polyhydroxy monocarboxylate is sodium gluconate.
  • the sequestrant may preferably be an organodiphosphonic acid selected from the group consisting of 1-hydroxyethane 1,1- diphosphonic acid (HEDP), amino tris(methylenephospho nic acid) (ATMP), ethylenediamine tetra(methylene phosphonic acid) (EDTMP), tetramethylenediamine tetra(methylene phosphonic acid) (TDTMP), hexamethylenediamine tetra(methylene phosphonic acid) (HDTMP), diethylenetriamine penta(methylene phosphonic acid) (DTPMP), and combinations thereof.
  • HEDP 1-hydroxyethane 1,1- diphosphonic acid
  • ATMP amino tris(methylenephospho nic acid)
  • ETMP ethylenediamine tetra(methylene phosphonic acid)
  • TTMP tetramethylenediamine tetra(methylene phosphonic acid)
  • HDTMP hexamethylenediamine tetra(methylene phosphonic acid)
  • the amount of the sequestrant in the co-granule ranges from 20 to 30 wt.%.
  • the co-granule comprises at least 25 wt.%, preferably at least 28 wt.%, still preferably at least 30 wt.% and most preferably at least 35 wt.%, but typically not more than 48 w.t%, still preferably not more than 45 wt.%, still further preferably not more than 43 wt.% and most preferably not more than 40 wt.%.
  • the weight ratio of the sequestrant to the total weight of the layering agent and the hydrating agent in the co-granule ranges from 1:1 to 1:4.
  • the active ingredient may be a hygroscopic cosurfactant preferably selected from the group consisting of amphoteric cosurfactant, sugar based cosurfactant, nonionic surfactant or mixtures thereof.
  • Cosurfactant refers to a surfactant that is a minor in the solid laundry detergent composition, and that preferably has an effect on primary detergency.
  • the cosurfactant can be a mixture of several cosurfactants.
  • the cosurfactant is typically a surfactant different from a anionic sulphonate surfactant, anionic sulphate surfactant, soap or mixtures thereof.
  • Particularly cosurfactant is typically a surfactant different from a linear alkyl benzene sulphonate (LAS).
  • LAS linear alkyl benzene sulphonate
  • the amphoteric cosurfactant is a betaine surfactant, still preferably CAPB.
  • the amount of amphoteric cosurfactant ranges from 10 wt.% to 35 wt.% in the co-granule. Still preferably the amount of the amphoteric cosurfactant ranges from 10 wt.% to 30 wt.%. Still preferably the amount of the amphoteric cosurfactant ranges from 12 wt.% to 35 wt.%.
  • the co-granule comprises at least 12 wt.%, preferably at least 14 wt.%, still preferably at least 15 wt.% and most preferably at least 18 wt.%, but typically not more than 20 w.t%, still preferably not more than 30 wt.%, still further preferably not more than 28 wt.% and most preferably not more than 25 wt.%.
  • amphoteric includes (a) surfactant molecules that contain both an acidic and basic site such as, for example, an amino acid containing both amino (basic) and acid (e.g., carboxylic acid, acidic) functional groups; or (b) zwitterionic surfactant molecules which possess both positive and negative charges within the same molecule.
  • the charges of the zwitterionic molecule may be either dependent or independent of the pH of the composition.
  • amphoteric surfactant as used herein, is also intended to encompass zwitterionic surfactants, which are well known to formulators skilled in the art as a subset of amphoteric surfactants.
  • Non-limiting examples of amphoteric surfactants useful in the compositions of the present invention are disclosed in McCutcheon's, Detergents and Emulsifiers, North American edition (1986), published by allured Publishing Corporation; and McCutcheons, Functional Materials, North American Edition (1992); both of which are incorporated by reference herein in their entirety.
  • amphoteric surfactants suitable for use in the present invention include, but are not limited to, amphocarboxylates such as alkylamphoacetates (mono or di); alkyl betaines; alkylamidoalkyl betaines; alkylamidoalkyl sultaines; alkyl amphophosphates; phosphorylated imidazolines such as phosphobetaines and pyrophosphobetaines; carboxyalkyl alkyl polyamines; alkylimino-dipropionates; alkylamphoglycinates (mono or di); alkyl amphopropionates (mono or di), ); N-alkyl [3-aminoproprionic acids; alkyl polyaminocarboxylates; and mixtures thereof.
  • amphocarboxylates such as alkylamphoacetates (mono or di); alkyl betaines; alkylamidoalkyl betaines; alkylamidoalkyl s
  • amphoteric surfactants include those given hereinbelow.
  • the amphoteric surfactant is preferably selected from the group consisting of betaines, sultaines, amine oxide or mixtures thereof.
  • a preferred amphoteric surfactant is the betaine type surfactant.
  • the amphoteric surfactant is Cocamidopropyl Betaine (CAPB).
  • the cocamidopropyl Betaine is commercially available from Rhone-Poulenc as Mirataine BDJ, Galaxy, Huntsman.
  • amphoteric surfactant are those which are broadly described as derivatives of aliphatic secondary and tertiary amines, preferably wherein the nitrogen is in a cationic state, in which the aliphatic radicals can be straight or branched chain and wherein one of the radicals contains an ionizable water solubilizing group, e.g., carboxy, sulfonate, sulfate, phosphate, or phosphonate.
  • an ionizable water solubilizing group e.g., carboxy, sulfonate, sulfate, phosphate, or phosphonate.
  • the amphoteric surfactant includes derivatives of aliphatic amines which contain a long chain of carbon atoms with 8 to 18 carbon atoms and an anionic water-solubilizing group selected from the group consisting of but not limited to carboxylate, sulfonate, or sulphate. Examples of the compounds falling within this definition are sodium-3-dodecylamino propane sulfonate and dodecyl dimethyl ammonium hexanoate.
  • Alkyl amine oxide wherein R 1 is typically C 6 to C 24 alkyl (saturated or unsaturated) or mixtures thereof. Preferably C8 to C 18 alkyl group, for example, C 12 to C 14 alkyl.
  • R2 and R3, which may be the same or different, are C 1 to C 3 alkyl or hydroxyalkyl groups, for example, methyl groups.
  • amphoteric surfactant includes those wherein the degree of ionisation varies as a function of pH of the medium it is in. These have an isoelectric point (IEP) in the range from 3.5 to 6.5.
  • IEP isoelectric point
  • Preferred amphoteric surfactant may also be selected from internally-neutralized derivatives of aliphatic quaternary ammonium and phosphonium and tertiary sulfonium compounds in which the aliphatic radical can be straight chain or branched, and wherein one of the aliphatic substituents contains from 8 to 18 carbon atoms and one contains an anionic water solubilizing group.
  • amphoteric surfactant is selected from the group consisting of betaines, sultaines, amine oxide, alkyl iminoacetates, imino dialkanoates, amino alkanoates alkyl ammonium propionates, or mixtures thereof. More preferably the amphoteric surfactant are betaines or amine oxide.
  • the betaine type amphoteric surfactant is selected from alkyl betaines, alkylamidoalkyl betaines and alkyl sulphobetaines.
  • the amine oxide type amphoteric surfactant is selected from alkyl amine oxide, alkylamidoalkyl amine oxide or mixtures thereof.
  • amphoteric surfactant is a cocamidopropyl betaine (CAPB).
  • the weight ratio of the amphoteric cosurfactant to the total weight of the layering agent and the hydrating agent in the co-granule ranges from 1:2 to 1:9, more preferably 1:2.3 to 1:5.
  • Sugar based cosurfactant Preferably hygroscopic sugar based cosurfactant is an alkyl polyglucoside.
  • Alkyl polyglucoside (APG) are nonionic surfactants that have a hydrophobic fatty alcohol portion and a hydrophilic glucoside portion.
  • the alkyl part of the alkyl polyglucoside has carbon atoms in the range from 8 to 16, more preferably from 10 to 14, furthermore preferably from 12 to 14.
  • the hydrophilic polyglucoside group containing from about 1.5 to 4, most preferably from 1.6 to 2.7 glucoside units.
  • the alkyl polyglucoside surfactant has a formula RO(R 1 O) t Z x wherein Z is a moiety derived from glucose R is an alkyl group that contains from 8 to 16 carbon atoms; R 1 is ethylene, propylene and/or glyceryl, t has a value which ranges from 0 to 10, most preferably 0 and where x is a number from 1.5 to 4 most preferably from 1.6 to 2.7.
  • the number x indicates the number of glucoside units in a particular alkylpolyglucoside surfactant.
  • x can only assume integral values.
  • the physical sample can be characterised by the average value of x and this average value can assume non-integral values.
  • the values of x are to be understood to be average values.
  • the hydrophobic group (R) can be attached at the 2-, 3- or 4-positions rather than at the 1 -position, (thus giving a glucosyl as opposed to a glucoside).
  • glucosides attachment through the 1 -position, i.e., glucosides
  • the additional glucoside units are predominately attached to the previous glucoside unit's 2-position. Attachment through the 3-, 4- and 6-positions can also occur.
  • the preferred alkoxide moiety is ethoxide.
  • Typical hydrophobic groups include alkyl groups, either saturated or unsaturated, branched or unbranched containing from 8 to 16, preferably from about 12 to about 14 carbon atoms.
  • Suitable examples of APG include cocoglucoside (commercially available as PLANTACARE® 818 UP; BASF), caprylyl/capryl gluycoside (commercially available as PLANTACARE® 810 UP; BASF) which both have carbon atoms from 8 to 16, lauryl glucoside (commercially available as PLANTACARE® 1200 UP) with carbon atoms from 8 to 16 and decyl glucoside (commercially available as PLANTACARE® 2000 UP) with carbon atoms in from 8 to 16.
  • the amount of sugar based cosurfactant ranges from 10 wt.% to 35 wt.% in the co- granule.
  • the amount of the sugar based cosurfactant ranges from 10 to 30 wt.%.
  • the co-granule comprises sugar based cosurfactant which is in an amount of at least 12 wt.%, preferably at least 14 wt.%, still preferably at least 15 wt.% and most preferably at least 18 wt.%, but typically not more than 20 w.t%, still preferably not more than 30 wt.%, still further preferably not more than 28 wt.% and most preferably not more than 25 wt.%.
  • the weight ratio of the sugar based cosurfactant to the total weight of the layering agent and the hydrating agent in the co- granule ranges from 1:2 to 1:9, more preferably 1:2.3 to 1:5.
  • Nonionic cosurfactant Preferably the nonionic surfactant is an alkoxylated nonionic surfactant, still preferably ethoxylated nonionic surfactant.
  • the ethoxylated nonionic surfactant has from 1EO group to 50 EO group, still preferably from 1EO to 20 EO group, still more preferably from 1EO to 10 EO, still more preferably from 1 EO to 7 EO group and most preferably from 1EO group to 3EO group.
  • the amount of nonionic surfactant ranges from 10 wt.% to 35 wt.% in the co-granule. Still preferably the amount of the nonionic cosurfactant ranges from 10 to 25 wt.%.
  • the co-granule comprises nonionic cosurfactant which is in an amount of at least 12 wt.%, preferably at least 14 wt.%, still preferably at least 15 wt.% and most preferably at least 18 wt.%, but typically not more than 20 w.t%, still preferably not more than 30 wt.%, still further preferably not more than 28 wt.% and most preferably not more than 25 wt.%.
  • the weight ratio of the nonionic cosurfactant to the total weight of the layering agent and the hydrating agent in the co-granule ranges from 1:2 to 1:9, more preferably 1:3 to 1:5.
  • the active ingredient may be a foam controlling agent.
  • the foam controlling agent may be selected preferably from a foam boosting agent, foam suppressing agent, foam optimizing agent or mixtures thereof.
  • a foam boosting agent includes those that increase the foam volume during the wash cycle and the rinse cycle.
  • the foam suppressing agent include those that decrease the foam volume during the wash and the rinse cycle.
  • the foam optimizing agent include those that increase the foam volume during the wash cycle but suppress or decrease the foam volume during the rinse cycle.
  • the foam suppressing agent is selected from the group consisting of silicone compound, amino silicone compound, glycerol derivative, diester compound, fatty acid, soap, polyols or combinations thereof.
  • the foam suppressing agent is selected from silicone compound, amino silicone compound, glycerol derivative, diester compound or mixtures thereof.
  • the foam suppressing agent is a delayed-release foam suppressing agent.
  • delayed release it is meant that the foam suppressing agent begins to suppress foam over time. The time delay may be adjusted depending on the time when the foam is required to be suppressed.
  • Silicone compound The foam suppressing agent may be a silicone compound.
  • the silicone compound includes a reactive siloxane structural unit comprising Si-O moieties where the reactive siloxane is a polymer which may include one or more functional moieties selected from the group amino, amido, alkoxy, hydroxy, polyether, carboxy, hydride, mercapto, sulfate phosphate and/or quaternary ammonium moieties.
  • These moieties may be attached directly to the siloxane backbone through a bivalent alkylene radical, (i.e., "pendant") or may be part of the backbone.
  • Suitable functionalized siloxane polymers include materials selected from the group consisting of aminosilicones, amidosilicones, silicone polyethers, silicone-urethane polymers, quaternary ABn silicones, amino ABn silicones, and combinations thereof.
  • the silicone compound is an organopolysiloxane preferably having an amino-functional or a carboxyl- functional organic group.
  • Suitable organosilicone may be linear, branched, or cross linked.
  • the silicone compound may belong to the organosiloxane class of amino amino-functional organopolysiloxane, carboxy-functional organopolysiloxane, polydimethyl siloxane, silicone polyether or mixtures thereof.
  • the silicone compound may also be selected from a reactive siloxane which is a silicone aminoalcohol. Yet another preferred silicone compound includes a reactive siloxane which is an aminosilicone.
  • the foam suppressing agent is an amino-functional organopolysiloxane (IV) which has at least one siloxane unit of the general formula and at least one siloxane unit of the general formula wherein: R 1 is the same or different and is a hydrogen atom, a monovalent, optionally fluorine-, chlorine- or bromine- substituted C 1 to C 18 hydrocarbyl radical or a C 1 to C 12 alkoxy radical or a hydroxyl radical, preferably a C 1 to C 18 hydrocarbyl radical or a C 1 to C3 alkoxy radical or a hydroxyl radical, where Q is an amino group of the general formula or forms thereof with partial or full protonation on the nitrogen atoms – NH 2 CH 2 CH 2 NH(CH 2
  • R 2 is a divalent C 1 to C 18 hydrocarbyl radical, preferably a divalent C2 to C4 hydrocarbyl radical hydrocarbyl radical
  • R 3 is a hydrogen atom or a C 1 to C 10 alkyl radical
  • R 4 is a hydrogen atom or a C 1 to C 10 alkyl radical
  • R 5 is a hydrogen atom or a C 1 to C 10 alkyl radical
  • a is 0, 1 or 2, preferably 0 or 1
  • b is 1, 2 or 3, preferably 1
  • c is 0, 1, 2 or 3, preferably 2 or 3
  • m is 2, 3 or 4, preferably 2 or 3
  • x is 0, 1 or 2, preferably 0 or 1, and the sum of a+b is less than or equal to 3.
  • the hydrocarbyl radical mentioned may be saturated or unsaturated, linear, branched or a cyclic radical.
  • the ratio of siloxane units with the general formula (IV a) to (IV b) is from 1:1 to 1:10,000 and preferably from 1:2 to 1:300.
  • the amino-functional organopolysiloxanes preferably have an average viscosity of 25 to 10,000 mPas, more preferably 50 to 5,000 mPas, at 25°C.
  • the foam suppressing agent is in solid form which includes an amino-functional organopolysilioxane of formula IV and a carrier material selected from the group of sodium carbonate, sodium sulphate, aluminium silicate, potassium carbonate, potassium sulphate, sodium hydrogencarbonate, potassium hydrogencarbonate and zeolites, and mixtures thereof.
  • a carrier material selected from the group of sodium carbonate, sodium sulphate, aluminium silicate, potassium carbonate, potassium sulphate, sodium hydrogencarbonate, potassium hydrogencarbonate and zeolites, and mixtures thereof.
  • Another preferred foam suppressing agent is a modified amino-functional organopolysilioxane have the general formula (V) where R2 is the same or different and is a monovalent C 1 to C 18 hydrocarbyl radical, R 1 is as defined above for (IVa) Q is as defined above for (IVa), k is 0 or 1, m is 0 or an integer from 1 to 1000, n is 0 or an integer from 1 to 50, with the proviso that the organopolysiloxanes contain at least one Q radical per molecule.
  • amino-functional organopolysiloxanes of the formula (V) are amino-functional polydimethylsiloxanes terminated by trimethylsiloxane units and amino-functional polydimethylsiloxanes terminated by hydroxydimethylsiloxane units and C 1 to C 3 alkoxydimethylsiloxane units.
  • A is an amino radical of the formula or a protonated amino form and/or acylated amino form of the amino radical A, preferably A is –(CH 2 ) 3 NH 2 and – (CH 2 ) 3 NH(CH 2 ) 2 NH 2 ;
  • X is a monovalent hydrocarbon radical having from 1 to 18 carbon atoms or a polyoxyalkylene group G of the formula preferably G is –(CH 2 ) 3 – (OC 2 H 4 ) y –O–R 6
  • R 1 is a C 1 to C 10 alkylene radical, preferably a radical of the formula -CH 2 CH 2 CH 2 -,
  • R 2 is hydrogen or a C 1 to C 4 alkyl radical, preferably hydrogen
  • R 3 is a C 1 to C 10 alkylene radical, preferably a radical of the formula -CH 2 CH 2 -
  • R 4 is a C 1
  • the modified amino silicone organopolysiloxane are generally a fluid and therefore need a carrier filler selected from the group comprising sodium carbonate, sodium sulphate, aluminum silicate, potassium carbonate, potassium sulphate, sodium bicarbonate, potassium bicarbonate and zeolites to form a free-flowing powder form.
  • Still another preferred type of modified amino silicone organopolysiloxane useful in the present invention is the one having the formula (VII) where: Y is an amino group of the general formula or the protonated or acylated amino forms of the amino group Y, R 1 is the same or different and is a monovalent C 1 to C 6 alkyl radical or a C 1 to C 6 alkoxy radical or a hydroxyl radical, R is a monovalent C 1 to C 6 alkyl radical, R 2 is a monovalent C2 to C 6 alkyl radical, R 3 is a C 1 to C 10 alkylene radical, R 4 is a hydrogen or a C 1 to C4 alkyl radical, R 5 and R 6 independently represent hydrogen or a C 1 to C4 alkyl radical, j is an integer from 0 to 3, k is an integer from 0 to 3, z is an integer from 1 to 500, n is an integer from 1 to 70, m is an integer from 1 to 10, v is an integer from 0 to 15, x
  • the amino radical Y is preferably –(CH 2 ) 3 NH 2 and –(CH 2 ) 3 NH(CH 2 ) 2 NH 2 and its protonated acylated form or its mixtures thereof.
  • These modified amino silicone organopolysiloxane are generally a fluid and therefore need a carrier filler.
  • the carrier filler is water-soluble with a water solubility of 50 to 500 g/L at 25°C. More preferably the carrier filler is selected from the group comprising sodium carbonate, sodium sulphate, aluminum silicate, potassium carbonate, potassium sulphate, sodium bicarbonate, potassium bicarbonate and zeolites, water soluble starch or mixtures thereof to form a free-flowing powder form.
  • silicone polyethers comprise a polydimethylsiloxane backbone with one or more polyoxyalkylene chains.
  • the polyoxyalkylene moieties may be incorporated in the polymer as pendent chains or as terminal blocks.
  • the foam suppressing agent may be polysiloxane having the structure: where R and R' are the same or different alkyl or aryl groups having from 1 to 6 carbon atoms; and x is an integer of at least 20.
  • the preferred polysiloxanes are polydimethylsiloxanes, where both R and R' are methyl groups.
  • the polysiloxanes usually have a molecular weight of from 500 to 200,000 and a kinematic viscosity of from 50 to 2 ⁇ 10 6 mm 2 sec -1 .
  • the polysiloxanes have a kinematic viscosity of from 5 ⁇ 10 2 to 5 ⁇ 10 4 mm 2 sec -1 , most preferably from 3 ⁇ 10 3 to 3 ⁇ 10 4 mm 2 sec -1 at 25°C.
  • the polysiloxane is generally end blocked with trimethylsilyl groups, but other end-blocking groups are also suitable.
  • silicone oils examples include silicone oils 47v 100, 47v 5000 and 47v 12500 available from Rhone Poulenc; Silcolapse 430 and Silicone EP 6508 available from ICI; Rhodosil 454 available from Rhone Poulenc; and Silkonol AK 100 available from Wacker.
  • the silicone compound is an organosilicones selected from polydimethylsiloxane, dimethicone, dimethiconol, dimethicone crosspolymer, phenyl trimethicone, alkyl dimethicone, lauryl dimethicone, stearyl dimethicone and phenyl dimethicone, octyl amidomethicone, cetyl amidomethicone. Still preferably the silicone compound is selected from polydimethylsiloxane, octyl amidomethicone, cetyl amidomethicone and mixtures thereof.
  • foam suppressing agent examples include those available under the names DC 200 Fluid, DC 1664, DC 349, DC 346G available from Dow Corning Corporation, Midland, MI, and those available under the trade names SF1202, SF1204, SF96, and Viscasil available from Momentive Silicones, Waterford, NY.
  • foam suppressing agent a further foam suppressing agent such as finely divided particulate silica may also be used in the composition of the present invention.
  • Any type of silica can be employed in the preparation of hydrophobic silica. Preferred examples are precipitated silica and pyrogenic silica which can be converted to a hydrophobic form. More preferably the foam suppressing agent includes a mixture of polydimethylsiloxane and silica.
  • the foam suppressing agent as disclosed in the present invention is preferably a cyclohexane polycarboxylic acid derivative of the formula (VIII) in which R 1 may be identical or different. It is selected from straight chain or branched C 1 to C 10 -alkyl or C 3 to C 8 -cycloalkyl; m is 0, 1, 2 or 3; n is 2, 3 or 4, and R is H or a straight chain or branched C 1 to C 30 alkyl, where at least one radical R is C 1 to C 30 alkyl.
  • R 1 may be identical or different. It is selected from straight chain or branched C 1 to C 10 -alkyl or C 3 to C 8 -cycloalkyl; m is 0, 1, 2 or 3; n is 2, 3 or 4, and R is H or a straight chain or branched C 1 to C 30 alkyl, where at least one radical R is C 1 to C 30 alkyl.
  • R 1 is an alkyl group selected from methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, sec-butyl, tert-butyl, n-pentyl, n-hexyl, n-octyl and 2-ethylhexyl.
  • the R is an alkyl radical which includes those already mentioned under R 1 and n-nonyl, isononyl, n-decyl, isodecyl, n-undecyl, isoundecyl, n-dodecyl, isododecyl, n-tridecyl, isotridecyl, stearyl, n-eicosyl, where at least one radical R is n-nonyl, isononyl, n-decyl, isodecyl, n-undecyl, isoundecyl, n- dodecyl, isododecyl, n-tridecyl, isotridecyl, stearyl, n-eicosyl.
  • the R is isononyl.
  • the cyclohexane polycarboxylic acid derivatives may be selected from mono-, di-, tri-, tetra esters and anhydrides of cyclohexane polycarboxylic acids. Preferably, all the carboxylic acid groups are esterified.
  • the cyclohexane polycarboxylic acid derivative is chosen from the group consisting of ring-hydrogenated mono- and dialkyl esters of phthalic acid, isophthalic acid and terephthalic acid, ring-hydrogenated mono-, di- and trialkyl esters of trimellitic acid, of trimesic acid and of hemimellitic acid, or mono-, di-, tri- and tetra alkyl esters of pyrromellitic acid, where the alkyl groups may be linear or branched and in each case have 1 to 30, preferably 2 to 10, particularly preferably 3 to 18, carbon atoms, and mixtures of two or more thereof.
  • the cyclohexane polycarboxylic acid derivative is an alkyl ester of cyclohexane-1,4- dicarboxylic acid, alkyl ester of cyclohexane-1,2-dicarboxylic acid, mixed esters of cyclohexane- 1,2-dicarboxylic acid with C 1 to C 13 alcohols, mixed esters of cyclohexane-1,3-dicarboxylic acid with C 1 to C 13 alcohols, mixed esters of cyclohexane-1,4-dicarboxylic acid with C 1 to C 13 alcohols, alkyl esters of cyclohexane-1, 3-dicarboxylic acid.
  • the cyclohexane polycarboxylic acid derivative is an alkyl ester of cyclohexane- 1,2-dicarboxylic acid as given in the formula below where R 3 and R 4 are mutually independently selected from branched and unbranched C 7 to C 12 alkyl residues.
  • C 7 to C 12 alkyl is selected from n-heptyl, 1-methylhexyl, 2-methylhexyl, 1-ethylpentyl, 2-ethylpentyl, 1-propylbutyl, 1-ethyl-2-methylpropyl, n-octyl, isooctyl, 2-ethylhexyl, n-nonyl, isononyl, 2-propylhexyl, n-decyl, isodecyl, 2-propylheptyl, n-undecyl, isoundecyl, n-dodecyl, isododecyl and the like.
  • C 7 to C 12 alkyl stands for n-octyl, n-nonyl, isononyl, 2-ethylhexyl, isodecyl, 2- propylheptyl, n-undecyl or isoundecyl.
  • residues R 3 and R 4 both stand for 2- ethylhexyl, isononyl or 2- propylheptyl.
  • the alkyl ester of cyclohexane-1,2-dicarboxylic acid is preferably selected from the group consisting of di(isobutyl) ester of cyclohexane-1, 2-dicarboxylic acid, di(2-ethylhexyl) ester of cyclohexane-1, 2-dicarboxylic acid, di(isononyl) ester of cyclohexane-1, 2-dicarboxylic acid.
  • Preferred ester groups are straight-chain or branched alkyl groups having 6 to 13 carbon atoms. Most preferably it is a di(isononyl) ester of cyclohexane-1, 2-dicarboxylic acid.
  • Diisononylcyclohexane-1, 2-dicarboxylate is commercially available under the name Hexamoll® DINCH (BASF AG).
  • the cyclohexane polycarboxylic acid derivatives are preferably prepared according to the process disclosed in WO 99/32427.
  • Glycerol derivative The foam suppressing agent is preferably a glycerol derivative.
  • the glycerol derivative has the general formula (IX) as mentioned herein below. wherein the R 1 is H or C 12 to C 18 saturated or unsaturated alkyl ester and R 2 is C 12 to C 18 saturated or unsaturated alkyl ester.
  • the glycerol derivative is preferably glycerol monooleate, glycerol dioleate, glycerol monostearate, glycerol distearate and mixtures thereof, preferably the glycerol derivative is a glycerol monostearate, glycerol monooleate or mixtures thereof. Most preferably the glycerol derivative is a glycerol monooleate.
  • the foam suppressing agent is a glycerol derivative used in combination with methyl cellulose.
  • glycerol monooleate is used in combination with methyl cellulose.
  • the ratio of glycerol derivative to methyl cellulose is at least 0.6, preferably at least 0.75, more preferably 1.
  • the ratio of glycerol derivative to methyl cellulose is at most 1, preferably at most 2, more preferably at most 5, even more preferably at most 7.
  • Other suitable foam suppressing agents include the monocarboxylic fatty acids and soluble salts thereof, which are described in US 2,954,347.
  • Other foam suppressing agents are described in EP-A-0210731 and EP-A-0210721.
  • the amount of foam suppressing agent ranges from 5 wt.% to 20 wt.% in the co- granule. Still preferably the amount of the foam suppressing agent ranges from 5 to 15 wt.%.
  • the co-granule comprises foam suppressing agent in an amount of at least 6 wt.%, preferably at least 8 wt.%, still preferably at least 10 wt.% and most preferably at least 12 wt.%, but typically not more than 15 w.t%, still preferably not more than 19 wt.%, still further preferably not more than 18 wt.% and most preferably not more than 17 wt.%.
  • the foam boosting agent may be a siloxane with a polyoxyalkylene group.
  • foam boosting siloxane with a polyoxyalkylene group as described in WO2020/074302 and incorporated herein by reference.
  • amount of foam boosting agent ranges from 5 wt.% to 20 wt.% in the co-granule.
  • amount of the foam suppressing agent ranges from 5 to 15 wt.%.
  • the co-granule comprises foam boosting agent which is in an amount of at least 6 wt.%, preferably at least 8 wt.%, still preferably at least 10 wt.% and most preferably at least 12 wt.%, but typically not more than 15 w.t%, still preferably not more than 19 wt.%, still further preferably not more than 18 wt.% and most preferably not more than 17 wt.%.
  • foam boosting agent which is in an amount of at least 6 wt.%, preferably at least 8 wt.%, still preferably at least 10 wt.% and most preferably at least 12 wt.%, but typically not more than 15 w.t%, still preferably not more than 19 wt.%, still further preferably not more than 18 wt.% and most preferably not more than 17 wt.%.
  • foam boosting agent which is in an amount of at least 6 wt.%, preferably at least 8 wt.%, still
  • the polymer includes those which are cleaning polymers such as anti- redeposition polymers, anti-greying polymers, dye transfer inhibiting polymer and soil release polymers.
  • the polymers include positively charged class of polymers such as polyethyleneimine (PEI) and its derivatives such as ethoxylated (PEI) polymers, propoxylated (PEI) polymers, polyamines, polyquats, polyglycerol quats, and other PEI derivatives,
  • PEI or PEIs are branched, spherical polymeric amines, and the molecular weight of the PEI or PEI salt used is from about 800 daltons to about 2 million Daltons.
  • the charge density of the PEI or PEI salt used is from about 15 meq/g to about 25 meq/g, more preferably from about 16 meq/g to about 20 meq/g.
  • preferred PEIs include the those commercially available in the SOKALAN® family of polymers available from BASF, e.g., SOKALAN® HP20.
  • the polymer may be a dye transfer inhibitor which includes polyvinyl pyrrolidone (PVP), and copolymers of N-vinylpyrrolidone and N-vinylimidazole (PVP/PVI), available commercially from BASF, as Sokalan (Trade Mark) HPSO and HP56 respectively.
  • the polymer may be a soil release polymer which includes multifunctional polyethylene imines and/or multifunctional diamines. These includes those commercially available from BASF under the tradename Sokalan® FIP20 and Sokalan® HP96.
  • the multifunctional polyethylene imines are typically ethoxylated polyethylene imines with a weight-average molecular weight Mw in the range from 3000 to 250000, preferably 5000 to 200000, more preferably 8000 to 100000, more preferably 8000 to 50000, more preferably 10000 to 30000, and most preferably 10000 to 20000 g/mol.
  • the multifunctional polyethylene imines have 80 wt% to 99 wt%, preferably 85 wt% to 99 wt%, more preferably 90 wt% to 98 wt%, most preferably 93 wt% to 97 wt% or 94 wt% to 96 wt% ethylene oxide side chains, based on the total weight of the materials.
  • Multifunctional diamines according to the present invention are typically ethoxylated C2 to C12 alkylene diamines, preferably hexamethylene diamine, which are further quaternized and optionally sulfated.
  • the multifunctional diamines have a weight- average molecular weight Mw in the range from 2000 to 10000, more preferably 3000 to 8000, and most preferably 4000 to 6000 g/mol.
  • the ethoxylated hexamethylene diamine may preferably be furthermore quaternized and sulfated, may be employed, which contains on average 10 to 50, preferably 15 to 40 and even more preferably 20 to 30 ethylene oxide (EO) groups per NH- functional group, and which preferably bears two cationic ammonium groups and two anionic sulfate groups.
  • the polymer may include an amphiphilic graft co-polymer.
  • a suitable amphiphilic graft co- polymer comprises (i) a polyethyelene glycol backbone; and (ii) and at least one pendant moiety selected from polyvinyl acetate, polyvinyl alcohol and mixtures thereof.
  • a suitable amphilic graft co-polymer is Sokalan® HP22, supplied from BASF.
  • the amount of polymer as the active ingredient present in the co-granule is in an amount ranging from 5 wt.% to 25 wt.%. Still preferably the amount of the polymer ranges from 10 wt.% to 22 wt.%.
  • the weight ratio of the polymer to the total weight of the layering agent and the hydrating agent in the co-granule ranges from 1:3 to 1:9, more preferably 1:3.5 to 1:5.
  • Layering agent According to the first aspect of the present invention the co-granule includes a layering agent.
  • the layering agent is selected from the group consisting of calcium carbonate, zeolite, precipitated silica, dolomite, and mixtures thereof. Still preferably the layering agent is selected from the group consisting of calcium carbonate, dolomite, zeolite, and mixtures thereof. Most preferably the layering agent is zeolite.
  • Typical zeolite builders include but are not limited to zeolite A, zeolite P, zeolite MAP and mixtures thereof.
  • Layering agent are known to a person skilled in the art.
  • the layering agent as used herein refers to those ingredient which are added to improve the granularity of the product and specifically those which prevent aggregation and/or caking.
  • the layering agent is an inorganic ingredient.
  • the layering agent preferably has a weight average particle size ranging from 1 micrometers to 30 micrometers. Still more preferably the layering agent has a weight average particle size ranging from 4 micrometers to 30 micrometers. Still preferably the layering agent has a weight average particle size ranging from 1 micrometers to 15 micrometers.
  • the layering agent has a particle size ranging from 1 micrometers to 10 micrometers.
  • the layering agent has a liquid carrying capacity minimum 25 gm nonionic surfactant(C12EO7)/100 gram of the layering agent to 200 gm nonionic surfactant (C12EO7)/100 gram of the layering agent.
  • the liquid carrying capacity is determined using the Nonionic surfactant(C12EO7) adsorption method.
  • Hydrating agent According to the first aspect of the present invention the co-granule includes a hydrating agent.
  • the hydrating agent is a salt that is capable of forming a hydrate.
  • the hydrating agent is selected from the group consisting of alkali metal salt of carbonate, bicarbonate, or sulphate.
  • the hydrating agent is selected from the group consisting of alkali metal salt of carbonate, alkali metal salt of bicarbonate, alkali metal salt of sulphate and mixtures thereof.
  • the hydrating agent is selected from sodium carbonate, sodium bicarbonate, sodium sulphate and mixtures thereof.
  • the hydrating agent forms a hydrate when mixed with the active ingredient.
  • the term hydrating agent as used herein refers to a salt which are capable of forming a hydrate, preferably when mixed with the active ingredient.
  • hydrating agent includes salt which are water-soluble.
  • the hydrating agent includes salt which are in a state which is partially hydrated or anhydrous.
  • the hydrating agent includes salt which have hydrates at 20°C.
  • the hydrating agent includes inorganic salt.
  • the inorganic salt are non-phosphate salts.
  • the hydrating agent is not a bleach.
  • the hydrating agent has a weight average particle size ranging from 30 to 150 micrometers. More preferably the weight average particle size ranges from 50 micrometers to 100 micrometers.
  • the weight ratio of the amount of the layering agent to the hydrating agent ranges from 1:2.5 to 1:19 based on the total weight of layering agent and the hydrating agent.
  • the layering agent is zeolite
  • the hydrating agent is sodium carbonate and preferably weight ratio of zeolite to sodium carbonate ranges from 1:2.5 to 1:19 in the mixture comprising zeolite and carbonate.
  • the present inventors have found that maintaining these ratio ranges are important to providing the co-granule with longer shelf-life period while remaining free-flowing.
  • the porosity of the carbonate helps absorb moisture and the carbonate hydrates to give strength to the co-granule and together with improving the free-flowing properties of the co-granule. It is preferred that the zeolite has an average particle size less than 10 micrometers to ensure maximum layering and forms a barrier to moisture ingress.
  • the weight ratio of the active ingredient to the total weight of the layering agent and the hydrating agent in the co-granule ranges from 1:1 to 1:9, more preferably from 1:2 to 1:9.
  • Process for preparing the co-granule includes the steps of: (i) obtaining a hydrating agent, a layering agent and an active ingredient wherein the active ingredient is either a solid having a moisture content ranging from 0 wt.% to 20 wt.% or a liquid having a viscosity less than 1000 millipascal second; (ii) homogeneously mixing the hydrating agent and the active ingredient to form a mixture; (iii) adding the layering agent to the mixture obtained in step (ii) to form a co-granule.
  • weight ratio of the amount of the layering agent to the hydrating agent ranges from 1:2.5 to 1:19 based on the total weight of layering agent and the hydrating agent present in the co-granule.
  • the mixing is preferably carried out in a plough shear mixer and the liquid active ingredient is sprayed onto the hydrating agent to form a mixture.
  • the active ingredient is mixed with the hydrating agent for 20 seconds to 60 seconds.
  • the spraying of the liquid is carried out using a flat spray nozzle with a maximum pressure of 7 bars.
  • the layering agent is homogeneously mixed with the mixture obtained in the previous step to form a co-granule.
  • the layering agent is mixed with the mixture preferably for 20 seconds to 60 seconds.
  • the active ingredient is selected from the group consisting of sequestrant, co- surfactant, polymer or derivatives thereof, foam controlling agent and mixtures thereof.
  • the liquid active ingredient according to the present invention does not encompass anionic surfactant selected from the group consisting of anionic sulphonate surfactant, anionic alkyl sulphate surfactant, soap, and mixtures thereof.
  • the active ingredient includes 0 wt.% anionic surfactant selected from the group consisting of anionic sulphonate surfactant, anionic alkyl sulphate surfactant, soap, and mixtures thereof.
  • the mixing is preferably carried out in a low shear mixer and the solid active ingredient is uniformly mixed with the hydrating agent to form a mixture.
  • Any low-shear mixture known in the art may be used for mixing and is preferably a drum mixer, concrete mixer, or a ribbon mixture.
  • the hydrating agent and the solid active ingredient is mixed for a period of 60 seconds to 120 seconds.
  • the layering agent is homogeneously mixed with the mixture obtained in the previous step to form a co-granule.
  • the active ingredient is selected from the group consisting of sequestrant, co-surfactant, polymer or derivatives thereof, foam controlling agent and mixtures thereof.
  • the solid active ingredient according to the present invention does not encompass anionic surfactant selected from the group consisting of anionic sulphonate surfactant, anionic sulphate surfactant, soap or mixtures thereof.
  • the active ingredient includes 0 wt.% anionic surfactant selected from anionic sulphonate surfactant, anionic sulphate surfactant, soap or mixtures thereof.
  • Detergent composition According to a third aspect of the present invention disclosed is a solid laundry detergent composition including the co-granule.
  • the laundry composition according to the first aspect of the present invention preferably includes from 10 wt.% to 25 wt.% detergency builder.
  • the laundry composition includes from 5 wt.% to 50 wt.% alkyl benzene sulphonate surfactant.
  • the laundry composition has a moisture content ranging from 2 wt.% to 4.5 wt.%.
  • the laundry detergent composition is prepared by a spray-drying process and the co-granule is post-dosed to the spray-dried detergent particle.
  • the laundry detergent composition comprises a base detergent particle and the co- granule according to the present invention.
  • the solid laundry detergent composition includes from 10 wt.% to 95 wt.% of the base detergent particle.
  • the solid laundry detergent composition includes from 0.5 wt.% to 30 wt.% of the co-granule, more preferably from 1 wt.% to 20 wt.% of the co-granule.
  • the co-granule is post-dosed to the base detergent particle to formulate the solid laundry detergent composition.
  • the base detergent particle has from 2 wt.% to 80 wt.% anionic surfactant, more preferably from 5 wt.% to 50 wt.% anionic surfactant.
  • the base detergent particle is a spray-dried detergent particle, preferably where the spray-dried detergent particle includes from 2 wt.% to 50 wt.% anionic surfactant. More preferably the spray-dried detergent particle has an equilibrium pH ranging from 6.5 to 9 when measured at 1 wt.% dilution in deionized water at 20°C, more preferably an equilibrium pH ranging from 6.5 to 8. More preferably the spray-dried detergent particle comprises a salt of organic carboxylic acid selected from organic carboxylic acid salt of Aluminium, organic carboxylic acid salt of alkaline earth metal, organic carboxylic acid salt of Aluminium or organic carboxylic acid salt of alkaline earth metal in combination with organic carboxylic acid salt of alkali metal and mixtures thereof.
  • the spray dried detergent particle includes 1 to 10 wt.% organic acid.
  • the spray-dried detergent particle includes in-situ formed silica.
  • the base detergent particle includes from 0 to 8 wt.% zeolite builder.
  • the base detergent particle includes from 0 to 4 wt.% phosphate builder.
  • the base detergent particle includes from 0 to 8 wt.% carbonate builder.
  • the base detergent particle includes from 0 to 8 wt.% sodium silicate.
  • a suitable spray-drying process involves the step of forming an aqueous slurry mixture, transferring it through at least one pump, preferably two pumps, to a pressure nozzle.
  • the spray drying tower is a counter-current spray drying tower, although a co-current spray-drying tower may also be suitable.
  • the spray-dried base detergent particle has a weight average particle size ranging from 300 micrometers to 500 micrometers and preferably less than 10 wt.% have a particle size greater than 2360 micrometers.
  • the base detergent particle is prepared by a mixing process.
  • the base detergent particle is an agglomerate detergent particle.
  • the agglomerate base detergent particle includes from 2 wt.% to 50 wt.% anionic surfactant, still more preferably from 4 wt.% to 35 wt.% anionic surfactant.
  • a suitable agglomeration process comprises the step of contacting a detersive ingredient, preferably an anionic surfactant, more preferably selected from the group consisting of sulphonate surfactant, alkyl sulphate surfactant, alkoxylated sulphate surfactant and mixtures thereof with an inorganic material in a mixer.
  • the anionic surfactant is linear alkyl benzene sulphonate surfactant (LAS) and/or alkyl sulphate surfactant and/or alkyl alkoxylated sulphate surfactant.
  • the inorganic material is selected from sodium carbonate, silica, silicate and mixtures thereof.
  • the agglomeration may include a step of in-situ neutralization agglomeration process where an acid precursor of the detersive surfactant, preferably anionic surfactant and particularly LAS is contacted with an alkaline material such as sodium carbonate, and/or sodium hydroxide in a mixer, and where the acid precursor of a detersive surfactant is neutralized by the alkaline material to form detersive surfactant during the agglomeration process.
  • the agglomeration process may be a high, medium or low shear agglomeration process, wherein a high shear, medium shear, low shear mixer is used accordingly.
  • the agglomeration process may be a multi-step agglomeration process wherein two or more mixers are used, such as a high shear mixer in combination with a medium or low shear mixer.
  • the agglomeration process can be a continuous process or a batch process.
  • the agglomerates have a particle size distribution such that weight average particle size is in the range of from 300 micrometers to 800 micrometers, and less than 10 wt.% of the agglomerates have particle size less than 150 micrometers and less than 10 wt.% of the agglomerates have a particle size greater than 1200 micrometers.
  • the solid laundry detergent composition includes a base detergent particle which is prepared by an extrusion process and the co-granule is post-dosed to the extruded base detergent particle.
  • the extruded base detergent particle is in various shapes and sizes and not limited to needles, flakes, rods, noodles and mixtures thereof.
  • the laundry detergent composition includes a mixture of one or more of the base detergent particle selected from spray-dried detergent particle, agglomerate detergent particle, extruded detergent particle, detergent particle in the form of needles, flakes, rods, noodles or mixtures thereof and the co-granule of the present invention.
  • the solid laundry detergent composition comprising the base detergent particle preferably having anionic surfactant and the co-granule according to the present invention was found to provide good product physical profile, and the composition has good powder characteristics and good anticaking properties even under extended storage periods.
  • the solid laundry detergent composition preferably includes optional ingredients which may be selected from the non-limiting examples consisting of bleach, shading dyes, brighteners, hueing agents, enzymes selected from amylase, cellulase, lipase, mannanase, xyloglucanase, cutinase, lyase, bleaching enzyme and mixtures thereof; perfume, visual cues and mixtures thereof. Examples Evaluation of the shelf life of co-granules with different amounts of the layering agent and the hydrating agent.
  • a co-granule having MGDA as the solid active ingredient with a moisture content of 5 wt.% was prepared by mixing the MGDA powder with sodium carbonate as the hydrating agent in a low shear mixer at a speed of 5 to 10 rpm for 120 seconds. After homogeneously mixing, zeolite was added as a layering agent and mixed to get a co-granule. Different co-granules were prepared with different levels of the hydrating agent and the layering agent as shown in table 1 below.
  • the shelf life of the different co- granules was determined.100 grams of the co-granule was placed in a sealed PET-PE laminate under hot humid conditions (40°C and 85% RH) and were evaluated at regular intervals of 30 days up to 12 weeks, to check for caking or lump formation. The co-granules were passed through a 50mm sieve and any lumps retained above the sieve were counted. If the number of lumps retained on the sieve was more than 10 then the co-granule was said to have caked and the study for that package was stopped and the shelf-life was recorded and provided in the table 1 below.
  • each of the different co-granule shown in table 1 was added into a laundry detergent composition having a composition as provided in table 2 below and the storage study test was repeated as described above to determine the shelf-life.
  • Table 1 The data in table 1 shows that the co-granule according to the present invention having a weight ratio between hydrating agent to a layering agent in the claimed ranges has a longer shelf life.
  • the comparative co-granule where either a layering or a hydrating agent is present (Ex A, Ex B) or where the weight ratio between the layering agent and the hydrating agent is outside the claimed range (Ex C) has shorter shelf life.
  • Table 2 The data in table 2 shows that when the co-granule (Ex 1) according to the present invention is incorporated into a spray-dried detergent composition having a weight ratio between hydrating agent to a layering agent is in the claimed ranges the solid laundry composition has a longer shelf life.

Abstract

La présente invention concerne une composition de détergent textile solide. Plus particulièrement, l'invention concerne une composition de détergent textile solide ayant une particule d'agent actif à écoulement libre. Un objet de la présente invention est donc de fournir un liquide ou un principe actif solide qui peut être incorporé dans une composition de détergent solide tout en conservant de bonnes propriétés de poudre. Un premier aspect de la présente invention concerne une composition de détergent textile solide comprenant un co-granule, le co-granule comprenant : (i) un principe actif, le principe actif étant un solide présentant une teneur en humidité allant de 0 % en poids à 20 % en poids, ou le principe actif étant un liquide présentant une viscosité inférieure à 1000 millipascals-seconde ; (ii) un agent de stratification ; (iii) un agent hydratant ; le principe actif étant intimement mélangé à l'agent hydratant et l'agent de stratification et le rapport pondéral de la quantité d'agent de stratification à l'agent hydratant allant de 1:2,5 à 1:19 dans le co-granule.
PCT/EP2023/070249 2022-07-29 2023-07-21 Composition de détergent textile WO2024022962A1 (fr)

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EP22187947 2022-07-29

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US2954347A (en) 1955-10-27 1960-09-27 Procter & Gamble Detergent composition
US3299112A (en) 1964-06-19 1967-01-17 Union Carbide Corp Siloxane wetting agents
EP0210721A2 (fr) 1985-07-25 1987-02-04 Dow Corning Limited Agents contrôlant la mousse pour détergents
EP0210731A2 (fr) 1985-07-25 1987-02-04 Dow Corning Limited Agents pour contrôler la mousse dans les détergents
US4818421A (en) 1987-09-17 1989-04-04 Colgate-Palmolive Co. Fabric softening detergent composition and article comprising such composition
WO1999006524A1 (fr) * 1997-07-30 1999-02-11 Basf Aktiengesellschaft Formulation detergente solide pour textiles a base de derives d'acide n,n-diacetique de glycine comme adjuvants a teneur fortement reduite en adjuvants au silicate
WO1999032427A1 (fr) 1997-12-19 1999-07-01 Basf Aktiengesellschaft Procede d'hydrogenation d'acides polycarboxyliques de benzene ou de leurs derives a l'aide d'un catalyseur a macropores
US20050098759A1 (en) 2000-09-07 2005-05-12 Frankenbach Gayle M. Methods for improving the performance of fabric wrinkle control compositions
US20180094225A1 (en) * 2016-10-03 2018-04-05 The Procter & Gamble Company Laundry detergent composition
WO2020074302A1 (fr) 2018-10-12 2020-04-16 Unilever N.V. Composition de nettoyage comprenant une silicone augmentant le pouvoir moussant
CN112500936A (zh) * 2020-12-11 2021-03-16 纳爱斯集团有限公司 洗衣粉及其生产工艺、造粒粉和造粒粉的造粒工艺

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US2954347A (en) 1955-10-27 1960-09-27 Procter & Gamble Detergent composition
US3299112A (en) 1964-06-19 1967-01-17 Union Carbide Corp Siloxane wetting agents
EP0210721A2 (fr) 1985-07-25 1987-02-04 Dow Corning Limited Agents contrôlant la mousse pour détergents
EP0210731A2 (fr) 1985-07-25 1987-02-04 Dow Corning Limited Agents pour contrôler la mousse dans les détergents
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WO2020074302A1 (fr) 2018-10-12 2020-04-16 Unilever N.V. Composition de nettoyage comprenant une silicone augmentant le pouvoir moussant
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