EP1276843B1 - Compositions en sachet - Google Patents

Compositions en sachet Download PDF

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Publication number
EP1276843B1
EP1276843B1 EP01916548A EP01916548A EP1276843B1 EP 1276843 B1 EP1276843 B1 EP 1276843B1 EP 01916548 A EP01916548 A EP 01916548A EP 01916548 A EP01916548 A EP 01916548A EP 1276843 B1 EP1276843 B1 EP 1276843B1
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EP
European Patent Office
Prior art keywords
water
composition
alkyl
compartment
acid
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.)
Expired - Lifetime
Application number
EP01916548A
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German (de)
English (en)
Other versions
EP1276843A2 (fr
Inventor
Nigel Patrick Somerville-Roberts
Bruno Matthieu Dasque
Thomas John Pounds
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.)
Procter and Gamble Co
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Procter and Gamble Co
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Publication date
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Publication of EP1276843A2 publication Critical patent/EP1276843A2/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
    • C11D17/04—Detergent materials or soaps characterised by their shape or physical properties combined with or containing other objects
    • 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
    • C11D17/04—Detergent materials or soaps characterised by their shape or physical properties combined with or containing other objects
    • C11D17/041—Compositions releasably affixed on a substrate or incorporated into a dispensing means
    • C11D17/042—Water soluble or water disintegrable containers or substrates containing cleaning compositions or additives for cleaning compositions
    • C11D17/043—Liquid or thixotropic (gel) compositions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D25/00—Details of other kinds or types of rigid or semi-rigid containers
    • B65D25/02—Internal fittings
    • B65D25/04—Partitions
    • B65D25/08—Partitions with provisions for removing or destroying, e.g. to facilitate mixing of contents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D81/00—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
    • B65D81/32—Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents for packaging two or more different materials which must be maintained separate prior to use in admixture
    • B65D81/3261—Flexible containers having several compartments
    • B65D81/3272—Flexible containers having several compartments formed by arranging one flexible container within another
    • 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
    • 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
    • C11D17/04—Detergent materials or soaps characterised by their shape or physical properties combined with or containing other objects
    • C11D17/041—Compositions releasably affixed on a substrate or incorporated into a dispensing means
    • C11D17/042—Water soluble or water disintegrable containers or substrates containing cleaning compositions or additives for cleaning compositions
    • C11D17/045—Multi-compartment
    • 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
    • C11D3/0005—Other compounding ingredients characterised by their effect
    • C11D3/0026—Low foaming or foam regulating compositions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • 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
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/386—Preparations containing enzymes, e.g. protease or amylase
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/39—Organic or inorganic per-compounds
    • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
    • C11D3/3905—Bleach activators or bleach catalysts
    • 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
    • C11D3/40—Dyes ; Pigments
    • C11D3/42—Brightening agents ; Blueing agents
    • 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
    • C11D3/43—Solvents
    • 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
    • C11D3/50—Perfumes

Definitions

  • This invention relates to a pouch having at least two compartments, said pouch comprises a composition comprising a solid component and a liquid component, said solid and liquid components are contained in different compartments.
  • Laundry detergent products can be found on the market to date in various forms, such as solid granular compositions and tablets, or liquid compositions. This gives the consumer a choice of detergent products they can use.
  • Some detergent ingredients currently used by the laundry industry are preferably manufactured and processed in solid form, for example because these ingredients are water-insoluble and are difficult or costly to include in a liquid detergent composition, or because these materials are preferably transported and supplied in solid form and therefore require extra processing steps to enable them to be included in a liquid detergent composition.
  • Such detergent ingredients include surfactants, hence these surfactants require extra processing steps to enable them to be included in liquid detergent compositions.
  • certain ingredients are formed into granular form and supplied and processed in solid form for stability reasons, for example certain enzyme prills.
  • liquid detergent compositions include the use of emulsifiers, and dispersants.
  • these liquid detergent compositions comprise only low amounts of these solid ingredients.
  • liquid detergent ingredients can comprise only low amounts of certain water-insoluble building agents such as aluminosilicates or water-insoluble fabric softening agents such as clays, provided dispersants or emulsifiers are used.
  • the inventors have found that by using a multi-compartment water-soluble pouch comprising at least two separate compartments, water-insoluble solid detergent ingredients can be included in a detergent composition comprising other liquid detergent ingredients, without the need for difficult, costly manufacturing and processing steps.
  • the water-insoluble solid detergent ingredient is comprised by one compartment of a multi-compartment water-soluble pouch whilst the liquid detergent ingredients are comprised by another compartment of said pouch.
  • Detergent compositions comprised by a multi-compartment water-soluble pouch in this way can comprise higher levels of water-insoluble solid detergent ingredients such as water insoluble building agent together with liquid detergent ingredients.
  • US 4 973 41 G describes an aqueous liquid laundry detergent preferably in a pouch or packet comprising from 10% to 24% by weight of water and a substantially organic neutralisation system.
  • EP 1 126 070 (state of the art under Art. 54(3) EPC) describes a two compartment pouch made using a substantially water soluble film or sheer made from hydroxyl propyl methyl cellulose.
  • a multi-compartment pouch made from a water-soluble film comprising a polyvinyl alcohol polymer and having at least two compartments, said multi-compartment pouch comprises a composition comprising a solid component and a liquid component, wherein;
  • the multi-compartment pouch of the invention herein referred to as "pouch", comprises at least two, preferably two compartments.
  • the pouch herein is typically a closed structure, made of material described herein, enclosing a volume space which is separated into at least two compartments.
  • the pouch comprises a composition comprising a liquid component and a solid component.
  • the pouch and volume space thereof can be of any form, shape and material which is suitable to hold the composition, e.g. without allowing the release of the composition from the pouch prior to contact of the pouch to water. The exact execution will depend on for example the type and amount of the composition in the pouch, the number of compartments in the pouch, the characteristics required from the pouch to hold, protect and deliver or release the compositions.
  • the pouch has a spheroid shape.
  • the pouch may be of such a size that it conveniently contains either a unit dose amount of the composition herein, suitable for the required operation, for example one wash, or only a partial dose, to allow the consumer greater flexibility to vary the amount used, for example depending on the size and/ or degree of soiling of the wash load.
  • the pouch is made from a water-soluble film which encloses an inner volume, said inner volume is divided into the compartments of the pouch.
  • the compartments of the pouch herein typically are closed structures made of a water-soluble film which encloses a volume space which comprises the components of the detergent composition. Said volume space is preferably enclosed by a water-soluble film in such a manner that the volume space is separated from the outside environment.
  • the solid component or liquid component that are comprised by a compartment of the pouch are contained in the volume space of the compartment, and are separated from the outside environment by a water-soluble film.
  • separated means for the purpose of this invention "physically distinct, in that a first ingredient comprised by a compartment is prevented from contacting a second ingredient if said second ingredient is not comprised by the same compartment which comprises said first ingredient".
  • outside environment means for the purpose of this invention "anything which cannot pass through the material which encloses the compartment and which is not comprised by the compartment".
  • the compartment is suitable to hold the solid or liquid components of the composition, e.g. without allowing the release of the components from the compartment prior to contact of the pouch to water.
  • the compartment can have any form or shape, depending on the nature of the material of the compartment, the nature of the components or composition, the intended use, amount of the components etc.
  • the compartment which comprises the liquid component also comprises an air bubble, preferably the air bubble has a volume of no more than 50%, preferably no more than 40%, more preferably no more than 30%, more preferably no more than 20%, more preferably no more than 10% of the volume space of said compartment.
  • the presence of the air bubble increases the tolerance of the pouch to the movement of liquid component within the compartment, thus reducing the risk of the liquid component leaking from the compartments.
  • the pouch is made from a water-soluble film, said water-soluble film typically has a solubility of at least 50%, preferably at least 75% or even at least 95%, as measured by the method set out hereinafter using a glass-filter with a maximum pore size of 50 microns, namely:
  • the films are polymeric materials which are formed into a film or sheet.
  • the material in the form of a film can for example be obtained by casting, blow-moulding, extrusion or blow extrusion of the polymer material, as known in the art.
  • the film comprises polyvinyl alcohol polymer (PVA).
  • the level of polymer in the film is at least 60%.
  • the polymer can have any weight average molecular weight, preferably from about 1000 to 1,000,000, or even from 10,000 to 300,000 or even from 15,000 to 200,000 or even from 20,000 to 150,000.
  • Mixtures of polymers can also be used. This may in particular be beneficial to control the mechanical and/or dissolution properties of the compartment or pouch, depending on the application thereof and the required needs. For example, it may be preferred that a mixture of polymers is present in the material of the compartment, whereby one polymer material has a higher water-solubility than another polymer material, and/or one polymer material has a higher mechanical strength than another polymer material.
  • a mixture of polymers is used, having different weight average molecular weights, for example a mixture of PVA or a copolymer thereof of a weight average molecular weight of 10,000- 40,000, preferably around 20,000, and of PVA or copolymer thereof, with a weight average molecular weight of about 100,000 to 300,000, preferably around 150,000.
  • polymer blend compositions for example comprising hydrolytically degradable and water-soluble polymer blend such as polylactide and polyvinyl alcohol, achieved by the mixing of polylactide and polyvinyl alcohol, typically comprising 1-35% by weight polylactide and approximately from 65% to 99% by weight polyvinyl alcohol, if the material is to be water-dispersible, or water-soluble.
  • hydrolytically degradable and water-soluble polymer blend such as polylactide and polyvinyl alcohol
  • the polymer present in the film is from 60-98% hydrolysed, preferably 80% to 90%, to improve the dissolution of the film.
  • Most preferred films are films which comprise a PVA polymer with similar properties to the film which comprises a PVA polymer and is known under the trade reference M8630, as sold by Chris-Craft Industrial Products of Gary, Indiana, US.
  • the film herein may comprise other additive ingredients than the polymer or polymer material.
  • plasticisers for example glycerol, ethylene glycol, diethyleneglycol, propylene glycol, sorbitol and mixtures thereof, additional water, disintegrating aids.
  • the composition herein is a detergent composition, that the film itself comprises a detergent additive to be delivered to the wash water, for example organic polymeric soil release agents, dispersants, dye transfer inhibitors.
  • the compartment and preferably pouch as a whole are made from water-soluble material.
  • Suitable examples of commercially available water-soluble materials include polyvinyl alcohol and partially hydrolysed polyvinyl acetate, alginates, cellulose ethers such as carboxymethylcellulose and methylcellulose, polyethylene oxide, polyacrylates and combinations of these.
  • the pouch herein comprises a composition, typically said composition is contained in the volume space of the pouch.
  • compositions are cleaning compositions or fabric care compositions, preferably hard surface cleaners, more preferably laundry or dish washing compositions including, pre-treatment or soaking compositions and other rinse additive compositions.
  • the composition herein comprises such an amount of a cleaning composition, that one or a multitude of the pouched compositions is or are sufficient for one wash.
  • the composition herein comprises at least one surfactant and at least one building agent.
  • the composition comprises a solid component and a liquid component.
  • a first compartment comprises the solid component and a second compartment comprises the liquid component, so that the solid component and liquid component are separated by a water-soluble films.
  • the solid component is comprised by a compartment of the pouch. Said compartment is a different compartment to the one that comprises the liquid component.
  • the solid component is substantially solid in that at least 90%, preferably at least 95%, more preferably at least 98% of the ingredients comprised by the solid component are in a solid form.
  • the solid component comprises ingredients that are either difficult or costly to include in a substantially liquid composition or that are typically transported and supplied as solid ingredients which require additional processing steps to enable them to be included in a substantially liquid composition.
  • Said solid component comprises (by weight of the solid component) at least 10%, more preferably at least 20%, more preferably at least 30%, more preferably at least 40%, more preferably at least 50%, more preferably at least 60%, more preferably at least 70%, more preferably at least 80% water-insoluble solid material.
  • Water-insoluble solid material is a water-insoluble building agent, the aluminosilicate, or water-insoluble fabric softening agents clay. Water-insoluble building agents are described in more detail hereinafter.
  • the solid component comprises (by weight of the solid component) at least 15%, or even at least 20%, or even at least 25%, or even at least 30%, or even at least 40%, or even at least 50%, or even at least 70% particles surfactant.
  • Said agglomerate particles comprise at least 20%, preferably at least 40%, more preferably at least 60%, more preferably at least 80%, more preferably at least 90%, more preferably at least 95% surfactant.
  • Typical surfactants for use in the present invention are described in more detail herein.
  • the particle may be of any form, for example an agglomerate, spray-dried particle, extrudate or for example a surfactant flake consisting essentially of surfactant.
  • Said solid component preferably comprises at least one additional ingredient selected from the group consisting of building agent, chelating agent, bleaching agent, bleach activator, enzyme or enzyme prill, brightener, suds suppressor and dye.
  • Said ingredients are in solid form, such as a particulate ingredient.
  • part or all of the ingredients of the solid component are not pre-granulated, such as agglomerated, spray-dried, extruded, prior to incorporation into the compartment, and that the component is a mixture of dry-mixed powder ingredients or even raw materials.
  • Preferred may be that for example less than 60% or even less than 40% or even less than 20% of the component is a free-flowable pre-granulated granules.
  • the liquid component is comprised by a compartment of the pouch. Said compartment is a different compartment to the one that comprises the solid component.
  • the liquid component is substantially liquid in that at least 90%, more preferably at least 95%, %, more preferably at least 98% ingredients comprised by the liquid component are in a liquid form at room temperature.
  • the liquid component preferably comprises (by weight of the liquid component) at least 1% water-soluble perfume.
  • the level of perfume comprised by the liquid composition is preferably at least 2%, more preferably at least 5%, more preferably at least 10%, more preferably at least 40%.
  • said liquid component comprises a solvent.
  • said solvent is an alcohol/water or alcohol based solvent, more preferably said solvent contains or consists of ethanol and/or n-butoxy propoxy propanol.
  • said liquid component comprises (by weight of liquid component) from 0.1% to 30%, more preferably from 5% to 25%, more preferably from 10% to 20% solvent.
  • the liquid component is substantially liquid (in that the liquid component comprises less than 10%, preferably less than 5%, more preferably less than 2% material in solid form at room temperature) and the solid component is substantially solid (in that the solid component comprises less than 10%, preferably less than 5%, more preferably less than 2% material in liquid form at room temperature).
  • ingredients that are difficult or costly to include in a composition comprising a substantial amount of liquid ingredients are comprised by the solid component.
  • the preferred amounts of ingredients described herein are % by weight of the whole composition and not % by weight of either the solid component or liquid component which comprise said ingredient.
  • composition herein especially the solid component of the composition herein preferably comprises a water-insoluble building agent.
  • water insoluble builders include the sodium aluminosilicates.
  • Suitable aluminosilicate zeolites have the unit cell formula Na z [(AlO 2 ) z (SiO 2 )y]. xH 2 O wherein z and y are at least 6; the molar ratio of z to y is from 1.0 to 0.5 and x is at least 5, preferably from 7.5 to 276, more preferably from 10 to 264.
  • the aluminosilicate material are in hydrated form and are preferably crystalline, containing from 10% to 28%, more preferably from 18% to 22% water in bound form.
  • the aluminosilicate zeolites can be naturally occurring materials, but are preferably synthetically derived. Synthetic crystalline aluminosilicate ion exchange materials are available under the designations Zeolite A, Zeolite B, Zeolite P, Zeolite X, Zeolite HS and mixtures thereof. Zeolite A has the formula: Na 12 [AlO 2 ) 12 (SiO 2 ) 12 ]. xH 2 O wherein x is from 20 to 30, especially 27. Zeolite X has the formula Na 86 [(AlO 2 ) 86 (SiO 2 ) 106 ]. 276 H 2 O.
  • Preferred crystalline layered silicates for use herein have the general formula: NaMSi X O 2X+1 .yH 2 O wherein M is sodium or hydrogen, x is a number from 1.9 to 4 and y is a number from 0 to 20.
  • Crystalline layered sodium silicates of this type are disclosed in EP-A-0164514 and methods for their preparation are disclosed in DE-A-3417649 and DE-A-3742043 .
  • x in the general formula above preferably has a value of 2, 3 or 4 and is preferably 2.
  • the most preferred material is ⁇ -Na 2 Si 2 0 5 , available from Hoechst AG as NaSKS-6.
  • the composition herein preferably comprises a water-insoluble fabric softening agents.
  • water-insoluble fabric softening agents include clays.
  • the water-insoluble fabric softening agents are cationic compounds.
  • Suitable cationic fabric softening agents include the water insoluble tertiary amines or dilong chain amide materials as disclosed in GB-A-1 514 276 and EP-B-0 011 1 340 .
  • these water-insoluble tertiary amines or dilong chain amide materials are comprised by the solid component of the composition herein.
  • any alkoxylated nonionic surfactants can be comprised by the composition herein, Those nonionic surfactants which are liquid at room temperature, are preferably included in the liquid component.
  • the ethoxylated and propoxylated nonionic surfactants arc preferred.
  • Preferred alkoxylated surfactants can be selected from the classes of the nomonic condensates of alkyl phenols, nonionic ethoxylated alcohols, nonionic ethoxylated/propoxylated fatty alcohols, nonionic ethoxylate/propoxylate condensates with propylene glycol, and the nonionic ethoxylate condensation products with propylene oxide ethylene diamine adducts.
  • nonionic alkoxylated alcohol surfactants being the condensation products of aliphatic alcohols with from 1 to 75 moles of alkylene oxide, in particular about 50 or from 1 to 15 moles, preferably to 11 moles, particularly ethylene oxide and/or propylene oxide, are highly preferred nonionic surfactants.
  • the alkyl chain of the aliphatic alcohol can either be straight or branched, primary or secondary, and generally contains from 6 to 22 carbon atoms.
  • Particularly preferred are the condensation products of alcohols having an alkyl group containing from 8 to 20 carbon atoms with from 2 to 9 moles and in particular 3 or 5 moles, of ethylene oxide per mole of alcohol.
  • Nonionic polyhydroxy fatty acid amide surfactant Nonionic polyhydroxy fatty acid amide surfactant
  • Polyhydroxy fatty acid amides are highly preferred nonionic surfactant comprised by the composition, in particular those having the structural formula R 2 CONR 1 Z wherein : R1 is H, C 1-18 , preferably C 1 -C 4 hydrocarbyl, 2-hydroxy ethyl, 2-hydroxy propyl, ethoxy, propoxy, or a mixture thereof, preferable C 1 -C 4 alkyl, more preferably C 1 or C 2 alkyl, most preferably C 1 alkyl (i.e., methyl); and R 2 is a C 5 -C 31 hydrocarbyl, preferably straight-chain C 5 -C 19 or C 7 -C 19 alkyl or alkenyl, more preferably straight-chain C 9 -C 17 alkyl or alkenyl, most preferably straight-chain C 11 -C 17 alkyl or alkenyl, or mixture thereof; and Z is a polyhydroxyhydrocarbyl having a linear hydrocarbyl chain with at least 3 hydroxyls directly connected to
  • a highly preferred nonionic polyhydroxy fatty acid amide surfactant for use herein is a C 12 -C 14 , a C 15 -C 17 and/or C 16 -C 18 alkyl N-methyl glucamide.
  • composition herein comprises a mixture of a C 12 -C 18 alkyl N-methyl glucamide and condensation products of an alcohol having an alkyl group containing from 8 to 20 carbon atoms with from 2 to 9 moles and in particular 3 or 5 moles, of ethylene oxide per mole of alcohol.
  • the polyhydroxy fatty acid amide can be prepared by any suitable process.
  • One particularly preferred process is described in detail in WO 9206984 .
  • a product comprising about 95% by weight polyhydroxy fatty acid amide, low levels of undesired impurities such as fatty acid esters and cyclic amides, and which is molten typically above about 80°C, can be made by this process.
  • Nonionic fatty acid amide surfactant Nonionic fatty acid amide surfactant
  • Fatty acid amide surfactants or alkoxylated fatty acid amides can also be comprised by the composition herein. They include those having the formula: R 6 CON(R 7 )(R 8 ) wherein R 6 is an alkyl group containing from 7 to 21, preferably from 9 to 17 carbon or even 11 to 13 carbon atoms and R 7 and R 8 are each individually selected from the group consisting of hydrogen, C 1 -C 4 alkyl, C 1 -C 4 hydroxyalkyl, and -(C 2 H 4 O) X H, where x is in the range of from 1 to 11, preferably 1 to 7, more preferably form 1-5, whereby it may be preferred that R 7 is different to R 8 , one having x being 1 or 2, one having x being from 3 to 11 or preferably 5.
  • Alkyl esters of fatty acids can also be comprised by the composition herein. They include those having the formula: R 9 COO(R 10 ) wherein R 9 is an alkyl group containing from 7 to 21, preferably from 9 to 17 carbon or even 11 to 13 carbon atoms and R 10 is a C 1 -C 4 alkyl, C C 1 -C 4 hydroxyalkyl, or -(C 2 H 4 O) X H, where x is in the range of from I to 11, preferably 1 to 7. more preferably form 1-5, whereby it may be preferred that R 10 is a methyl or ethyl group.
  • Alkylpolysaccharides can also be comprised by the composition herein, such as those disclosed in US Patent 4,565,647, Llenado, issued January 21, 1986 , having a hydrophobic group containing from 6 to 30 carbon atoms and a polysaccharide, e.g., a polyglycoside, hydrophilic group containing from 1.3 to 10 saccharide units.
  • Preferred alkylpolyglycosides have the formula R 2 O(C n H 2n O)t(glycosyl) X wherein R 2 is selected from the group consisting of alkyl, alkylphenyl, hydroxyalkyl, hydroxyalkylphenyl, and mixtures thereof in which the alkyl groups contain from 10 to 18 carbon atoms; n is 2 or 3; t is from 0 to 10, and x is from 1.3 to 8.
  • the glycosyl is preferably derived from glucose.
  • composition herein may comprise polyethylene and/or propylene glycol, particularly those of molecular weight 1000-10000, more particularly 2000 to 8000 and most preferably about 4000.
  • the composition herein preferably comprises one or more anionic surfactants.
  • Any anionic surfactant useful for detersive purposes is suitable. Examples include salts (including, for example, sodium, potassium, ammonium, and substituted ammonium salts such as mono-, di- and triethanolamine salts) of the anionic sulphate, sulphonate, carboxylate and sarcosinate surfactants. Anionic sulphate surfactants are preferred.
  • anionic surfactants include the isethionates such as the acyl isethionates, N-acyl taurates, fatty acid amides of methyl tauride, alkyl succinates and sulfosuccinates, monoesters of sulfosuccinate (especially saturated and unsaturated C 12 -C 18 monoesters) diesters of sulfosuccinate (especially saturated and unsaturated C 6 -C 14 diesters), N-acyl sarcosinates.
  • Resin acids and hydrogenated resin acids are also suitable, such as rosin, hydrogenated rosin, and resin acids and hydrogenated resin acids present in or derived from tallow oil.
  • Anionic sulphate surfactants suitable for use herein include the linear and branched primary and secondary alkyl sulphates, alkyl ethoxysulphates, fatty oleoyl glycerol sulphates, alkyl phenol ethylene oxide ether sulphates, the C 5 -C 17 acyl-N-(C 1 -C 4 alkyl) and -N-(C 1 -C 2 hydroxyalkyl) glucamine sulphates, and sulphates of alkylpolysaccharides such as the sulphates of alkylpolyglucoside (the nonionic non-sulphated compounds being described herein).
  • Alkyl sulphate surfactants are preferably selected from the linear and branched primary C 9 -C 22 acyl sulphates, more preferably the C 11 -C 15 branched chain alkyl sulphates and the C 12 -C 14 linear chain alkyl sulphates.
  • Alkyl ethoxysulfate surfactants are preferably selected from the group consisting of the C 10 -C 18 Alkyl sulphates which have been ethoxylated with from 0.5 to 50 moles of ethylene oxide per molecule. More preferably, the alkyl ethoxysulfate surfactant is a C 11 -C 18 , most preferably C 11 -C 15 alkyl sulphate which has been ethoxylated with from 0.5 to 7, preferably from I to 5, moles of ethylene oxide per molecule.
  • Anionic sulphonate surfactants suitable for use herein include the salts of C 5 -C 20 linear or branched alkylbenzene sulphonates, alkyl ester sulphonates, in particular methyl ester sulphonates, C 6 -C 22 primary or secondary alkane sulphonates, C 6 -C 24 olefin sulphonates, sulphonated polycarboxylic acids, alkyl glycerol sulphonates, fatty acyl glycerol sulphonates, fatty oleyl glycerol sulphonates, and any mixtures thereof.
  • Suitable anionic carboxylate surfactants include the alkyl ethoxy carboxylates, the alkyl polyethoxy polycarboxylate surfactants and the soaps ('alkyl carboxyls'), especially certain secondary soaps as described herein.
  • Suitable alkyl ethoxy carboxylates include those with the formula RO(CH 2 CH 2 0) X CH 2 C00 - M + wherein R is a C 6 to C 18 alkyl group, x ranges from O to 10, and the ethoxylate distribution is such that, on a weight basis, the amount of material where x is 0 is less than 20 % and M is a cation.
  • Suitable alkyl polyethoxy polycarboxylate surfactants include those having the formula RO-(CHR 1 -CHR 2 -O) X -R 3 wherein R is a C 6 to C 18 alkyl group, x is from I to 25, R 1 and R 2 are selected from the group consisting of hydrogen, methyl acid radical, succinic acid radical, hydroxysuccinic acid radical, and mixtures thereof, and R 3 is selected from the group consisting of hydrogen, substituted or unsubstituted hydrocarbon having between 1 and 8 carbon atoms, and mixtures thereof.
  • Suitable soap surfactants include the secondary soap surfactants which contain a carboxyl unit connected to a secondary carbon.
  • Preferred secondary soap surfactants for use herein are water-soluble members selected from the group consisting of the water-soluble salts of 2-methyl-l-undecanoic acid, 2-ethyl-l-decanoic acid, 2-propyl-l-nonanoic acid, 2-butyl-1-octanoic acid and 2-pentyl-1-heptanoic acid. Certain soaps may also be included as suds suppressers.
  • alkali metal sarcosinates of formula R-CON (R 1 )CH 2 COOM, wherein R is a C 5 -C 17 linear or branched alkyl or alkenyl group, R 1 is a C 1 -C 4 alkyl group and M is an alkali metal ion.
  • R is a C 5 -C 17 linear or branched alkyl or alkenyl group
  • R 1 is a C 1 -C 4 alkyl group
  • M is an alkali metal ion.
  • Another preferred surfactant is a cationic surfactant, which may preferably be present at a level of from 0.1% to 60% by weight of the composition herein, more preferably from 0.4% to 20%, most preferably from 0.5% to 5% by weight.
  • the ratio of the anionic surfactant to the cationic surfactant is preferably from 35:1 to 1:3, more preferably from 15: to 1:1. most preferably from 10:1 to 1:1.
  • the cationic surfactant is selected from the group consisting of cationic ester surfactants, cationic mono-alkoxylated amine surfactants, cationic bis-alkoxylated amine surfactants and mixtures thereof.
  • Preferred cationic mono-alkoxylated amine surfactant for use herein has the general formula: wherein R 1 is an alkyl or alkenyl moiety containing from about 6 to about 18 carbon atoms, preferably 6 to about 16 carbon atoms, most preferably from about 6 to about 11 carbon atoms; R 2 and R 3 are each independently alkyl groups containing from one to about three carbon atoms, preferably methyl; R 4 is selected from hydrogen (preferred), methyl and ethyl, X- is an anion such as chloride, bromide, methylsulphate, sulphate, or the like, to provide electrical neutrality; A is selected from C 1 -C 4 alkoxy, especially ethoxy (i.e., -CH 2 CH 2 O-), propoxy, butoxy and mixtures thereof; and p is from I to about 30, preferably I to about 15, most preferably 1 to about 8.
  • Highly preferred cationic mono-alkoxylated amine surfactants for use herein are of the formula: wherein R 1 is C 6 -C 18 hydrocarbyl and mixtures thereof, preferably C 6 -C 14 , especially C 6 -C 11 alkyl, preferably C 8 and C 10 alkyl, and X is any convenient anion to provide charge balance, preferably chloride or bromide.
  • compounds of the foregoing type include those wherein the ethoxy (CH 2 CH 2 O) units (EO) are replaced by butoxy, isopropoxy [CH(CH 3 )CH 2 O] and [CH 2 CH(CH 3 )O] units (i-Pr) or n-propoxy units (Pr), or mixtures of EO and/or Pr and/or i-Pr units.
  • the cationic bis-alkoxylated amine surfactant for use herein has the general formula: wherein R 1 is an alkyl or alkenyl moiety containing from about 6 to about 18 carbon atoms, preferably 6 to about 16 carbon atoms, more preferably 6 to about 11, most preferable from about 8 to about 10 carbon atoms; R 2 is an alkyl group containing from one to three carbon atoms, preferably methyl; R 3 and R 4 can vary independently and are selected from hydrogen (preferred), methyl and ethyl, X - is an anion such as chloride, bromide, methylsulphate, sulphate, or the like, sufficient to provide electrical neutrality.
  • a and A' can vary independently and are each selected from C 1 -C 4 alkoxy, especially ethoxy, (i.e., -CH 2 CH 2 O-), propoxy, butoxy and mixtures thereof; p is from 1 to about 30, preferably 1 to about 4 and q is from 1 to about 30, preferably 1 to about 4, and most preferably both p and q are 1.
  • Highly preferred cationic bis-alkoxylated amine surfactants for use herein are of the formula: wherein R 1 is C 6 -C 18 hydrocarbyl and mixtures thereof, preferably C 6 , C 8 , C 10 , C 12, C 14 alkyl and mixtures thereof.
  • X is any convenient anion to provide charge balance, preferably chloride.
  • cationic bis-alkoxylated amine surfactants useful herein include compounds of the formula: wherein R 1 is C 6 -C 18 hydrocarbyl, preferably C 6 -C 14 alkyl, independently p is 1 to about 3 and q is 1 to about 3, R 2 is C 1 -C 3 alkyl, preferably methyl, and X is an anion, especially chloride or bromide.
  • Suitable amphoteric surfactants for use herein include the amine oxide surfactants and the alkyl amphocarboxylic acids.
  • Suitable amine oxides include those compounds having the formula R 3 (OR 4 ) X NO(R 5 ) 2 wherein R 3 is selected from an alkyl, hydroxyalkyl, acylamidopropoyl and alkyl phenyl group, or mixtures thereof, containing from 8 to 26 carbon atoms; R 4 is an alkylene or hydroxyalkylene group containing from 2 to 3 carbon atoms, or mixtures thereof; x is from 0 to 5, preferably from 0 to 3; and each R 5 is an alkyl or hydroxyalkyl group containing from 1 to 3, or a polyethylene oxide group containing from 1 to 3 ethylene oxide groups.
  • Preferred are C 10 -C 18 alkyl dimethylamine oxide, and C 10-18 acylamido alkyl dimethylamine oxide.
  • a suitable example of an alkyl aphodicarboxylic acid is Miranol(TM) C2M Conc. manufactured by Miranol, Inc., Dayton, NJ.
  • Zwitterionic surfactants can also be comprised by the composition herein. These surfactants can be broadly described as derivatives of secondary and tertiary amines, derivatives of heterocyclic secondary and tertiary amines, or derivatives of quaternary ammonium, quaternary phosphonium or tertiary sulfonium compounds. Betaine and sultaine surfactants are exemplary zwitterionic surfactants for use herein.
  • Suitable betaines are those compounds having the formula R(R') 2 N + R 2 COO- wherein R is a C 6 -C 18 hydrocarbyl group, each R 1 is typically C 1 -C 3 alkyl, and R 2 is a C 1 -C 5 hydrocarbyl group.
  • Preferred betaines are C 12-18 dimethyl-ammonio hexanoate and the C 10-18 acylamidopropane (or ethane) dimethyl (or diethyl) betaines.
  • Complex betaine surfactants are also suitable for use herein.
  • composition herein may comprise a water-soluble building agent, typically present at a level of from 0% to 36% by weight, preferably from 1% to 35% by weight, more preferably from 10% to 35%, even more preferably from 12% to 30% by weight of the composition or particle.
  • a water-soluble building agent typically present at a level of from 0% to 36% by weight, preferably from 1% to 35% by weight, more preferably from 10% to 35%, even more preferably from 12% to 30% by weight of the composition or particle.
  • the water-soluble builder compound is an alkali or earth alkali metal salt of phosphate present at the level described above.
  • typical water-soluble building agents include the water soluble monomeric polycarboxylates, or their acid forms, homo or copolymeric polycarboxylic acids or their salts in which the polycarboxylic acid comprises at least two carboxylic radicals separated from each other by not more that two carbon atoms, borates, phosphates, and mixtures of any of the foregoing.
  • the carboxylate or polycarboxylate builder can be monomeric or oligomeric in type although monomeric polycarboxylates are generally preferred for reasons of cost and performance.
  • Suitable carboxylates containing one carboxy group include the water soluble salts of lactic acid, glycolic acid and ether derivatives thereof.
  • Polycarboxylates containing two carboxy groups include the water-soluble salts of succinic acid, malonic acid, (ethylenedioxy) diacetic acid, maleic acid, diglycolic acid, tartaric acid, tartronic acid and fumaric acid, as well as the ether carboxylates and the sulfinyl carboxylates.
  • Polycarboxylates containing three carboxy groups include, in particular, water-soluble citrates, aconitrates and citraconates as well as succinate derivatives such as the carboxymethyloxysuccinates described in British Patent No.
  • Polycarboxylates containing four carboxy groups include oxydisuccinates disclosed in British Patent No. 1,261,829 , 1,1,2,2-ethane tetracarboxylates, 1,1,3,3-propane tetracarboxylates and 1,1,2,3-propane tetracarboxylates.
  • Polycarboxylates containing sulfo substituents include the sulfosuccinate derivatives disclosed in British Patent Nos. 1,398,421 and 1,398,422 and in US Patent No. 3,936,448 , and the sulphonated pyrolysed citrates described in British Patent No. 1,439,000 .
  • Preferred polycarboxylates are hydroxycarboxylates containing up to three carboxy groups per molecule, more particularly citrates.
  • Suitable examples of water-soluble phosphate builders are the alkali metal tripolyphosphates, sodium, potassium and ammonium pyrophosphate, sodium and potassium and ammonium pyrophosphate, sodium and potassium orthophosphate, sodium polymeta/phosphate in which the degree of polymerization ranges from about 6 to 21, and salts of phytic acid.
  • a perhydrate bleach such as salts of percarbonates, particularly the sodium salts, and/ or organic peroxyacid bleach precursor. It has been found that when the pouch or compartment is formed from a material with free hydroxy groups, such as PVA, the preferred bleaching agent comprises a percarbonate salt and is preferably free form any perborate salts or borate salts. It has been found that borates and perborates interact with these hydroxy-containing materials and reduce the dissolution of the materials and also result in reduced performance.
  • Inorganic perhydrate salts are a preferred source of peroxide.
  • these salts are present at a level of from 0.01% to 50% by weight, more preferably of from 0.5% to 30% by weight of the composition or component.
  • inorganic perhydrate salts include percarbonate, perphosphate, persulfate and persilicate salts.
  • the inorganic perhydrate salts are normally the alkali metal salts.
  • the inorganic perhydrate salt may be included as the crystalline solid without additional protection.
  • the preferred executions of such granular compositions utilize a coated form of the material which provides better storage stability for the perhydrate salt in the granular product.
  • Suitable coatings comprise inorganic salts such as alkali metal silicate, carbonate or borate salts or mixtures thereof, or organic materials such as waxes, oils, or fatty soaps.
  • Alkali metal percarbonates particularly sodium percarbonate are preferred perhydrates herein.
  • Sodium percarbonate is an addition compound having a formula corresponding to 2Na 2 CO 3 .3H 2 O 2 , and is available commercially as a crystalline solid.
  • Potassium peroxymonopersulfate is another inorganic perhydrate salt of use in the compositions herein.
  • the composition herein preferably comprises a bleach activator, preferably comprising an organic peroxyacid bleach precursor. It may be preferred that the composition comprises at least two peroxy acid bleach precursors, preferably at least one hydrophobic peroxyacid bleach precursor and at least one hydrophilic peroxy acid bleach precursor, as defined herein.
  • the production of the organic peroxyacid occurs then by an in situ reaction of the precursor with a source of hydrogen peroxide.
  • the bleach activator may alternatively, or in addition comprise a preformed peroxy acid bleach.
  • At least one of the bleach activators preferably a peroxy acid bleach precursor having an average particle size, by weight, of from 600 microns to 1400 microns, preferably from 700 microns to 1100 microns is present in the composition herein.
  • At least 80%, preferably at least 90% or even at least 95 % or even substantially 100% of the component or components comprising the bleach activator have a particle size of from 300 microns to 1700 microns, preferably from 425 microns to 1400 microns.
  • the hydrophobic peroxy acid bleach precursor preferably comprises a compound having a oxy-benzene sulphonate group, preferably NOBS, DOBS, LOBS and/ or NACA-OBS, as described herein.
  • the hydrophilic peroxy acid bleach precursor preferably comprises TAED, as described herein.
  • the composition herein preferably comprises an organic peroxyacid precursor.
  • the production of the organic peroxyacid may occur by an in situ reaction of such a precursor with the percarbonate source.
  • a pre-formed organic peroxyacid is incorporated directly into the composition.
  • Peroxyacid bleach precursors are compounds which react with hydrogen peroxide in a perhydrolysis reaction to produce a peroxyacid.
  • peroxyacid bleach precursors may be represented as: where L is a leaving group and X is essentially any functionality, such that on perhydrolysis the structure of the peroxyacid produced is:
  • Suitable peroxyacid bleach precursor compounds typically contain one or more N- or O-acyl groups, which precursors can be selected from a wide range of classes.
  • Suitable classes include anhydrides, esters, imides, lactams and acylated derivatives of imidazoles and oximes. Examples of useful materials within these classes are disclosed in GB-A-1586789 .
  • Suitable esters are disclosed in GB-A-836988 , 864798 , 1147871 , 2143231 and EP-A-0170386 .
  • L group The leaving group, hereinafter L group, must be sufficiently reactive for the perhydrolysis reaction to occur within the optimum time frame (e.g., a wash cycle). However, if L is too reactive, this activator will be difficult to stabilize for use herein.
  • Preferred L groups are selected from the group consisting of: and mixtures thereof, wherein R 1 is an alkyl, aryl, or alkaryl group containing from 1 to 14 carbon atoms, R 3 is an alkyl chain containing from 1 to 8 carbon atoms, R 4 is H or R 3 , and Y is H or a solubilizing group. Any of R 1 , R 3 and R 4 may be substituted by essentially any functional group including, for example alkyl, hydroxy, alkoxy, halogen, amine, nitrosyl, amide and ammonium or alkyl ammonium groups.
  • the preferred solubilizing groups are -SO 3 - M + , -CO 2 - M + , -SO 4 - M + , -N + (R 3 ) 4 X - and O ⁇ --N(R 3 ) 3 and most preferably -SO 3 - M + and -CO 2 - M + wherein R 3 is an alkyl chain containing from 1 to 4 carbon atoms, M is a cation which provides solubility to the bleach activator and X is an anion which provides solubility to the bleach activator.
  • M is an alkali metal, ammonium or substituted ammonium cation, with sodium and potassium being most preferred, and X is a halide, hydroxide, methylsulphate or acetate anion.
  • Amide substituted alkyl peroxyacid precursor compounds are suitable herein, including those of the following general formulae: wherein R 1 is an alkyl group with from 1 to 14 carbon atoms, R 2 is an alkylene group containing from 1 to 14 carbon atoms, and R 5 is H or an alkyl group containing 1 to 10 carbon atoms and L can be essentially any leaving group.
  • Amide substituted bleach activator compounds of this type are described in EP-A-0170386 .
  • the organic peroxyacid bleaching system may contain a pre-formed organic peroxyacid.
  • a preferred class of organic peroxyacid compounds are the amide substituted compounds of the following general formulae: wherein R 1 is an alkyl, aryl or alkaryl group with from 1 to 14 carbon atoms, R 2 is an alkylene, arylene, and alkarylene group containing from 1 to 14 carbon atoms, and R 5 is H or an alkyl, aryl, or alkaryl group containing 1 to 10 carbon atoms.
  • Amide substituted organic peroxyacid compounds of this type are described in EP-A-0170386 .
  • organic peroxyacids include diacyl and tetraacylperoxides, especially diperoxydodecanedioc acid, diperoxytetradecanedioc acid and diperoxyhexadecanedioc acid.
  • diacyl and tetraacylperoxides especially diperoxydodecanedioc acid, diperoxytetradecanedioc acid and diperoxyhexadecanedioc acid.
  • Mono- and diperazelaic acid, mono- and diperbrassylic acid and N-phthaloylaminoperoxicaproic acid are also suitable herein.
  • composition herein preferably comprises as an optional ingredient, a chelating agent or heavy metal ion sequestrant.
  • heavy metal ion sequestrant it is meant herein components which act to sequester (chelate) heavy metal ions. These components may also have calcium and magnesium chelation capacity, but preferentially they show selectivity to binding heavy metal ions such as iron, manganese and copper.
  • Heavy metal ion sequestrants are generally present at a level of from 0.05% to 2%, preferably from 0.1% to 1.5%, more preferably from 0.25% to 1.2% and most preferably from 0.5% to 1% by weight of the composition herein.
  • Suitable heavy metal ion sequestrants for use herein include organic phosphonates; such as the amino alkylene poly (alkylene phosphonates), alkali metal ethane 1-hydroxy bisphosphonates and nitrilo trimethylene phosphonates.
  • Preferred among the above species are diethylene triamine penta (methylene phosphonate), ethylene diamine tri (methylene phosphonate) hexamethylene diamine tetra (methylene phosphonate) and hydroxy-ethylene 1,1 diphosphonate.
  • Suitable heavy metal ion sequestrant for use herein include nitrilotriacetic acid and polyaminocarboxylic acids such as ethylenediaminotetracetic acid, ethylenetriamine pentacetic acid, ethylenediamine disuccinic acid, ethylenediamine diglutaric acid, 2-hydroxypropylenediamine disuccinic acid or any salts thereof.
  • Suitable heavy metal ion sequestrants for use herein are iminodiacetic acid derivatives such as 2-hydroxyethyl diacetic acid or glyceryl imino diacetic acid, described in EP-A-317,542 and EP-A-399,133 .
  • iminodiacetic acid-N-2-hydroxypropyl sulfonic acid and aspartic acid N-carboxymethyl N-2-hydroxypropyl-3-sulfonic acid sequestrants described in EP-A-516,102 are also suitable herein.
  • EP-A-476,257 describes suitable amino based sequestrants.
  • EP-A-510,331 describes suitable sequestrants derived from collagen, keratin or casein.
  • EP-A-528,859 describes a suitable alkyl iminodiacetic acid sequestrant. Dipicolinic acid and 2-phosphonobutane-1,2.4-tricarboxylic acid are also suitable.
  • Glycinamide-N,N'-disuccinic acid (GADS), ethylenediamine-N-N'-diglutaric acid (EDDG) and 2-hydroxypropylenediamine-N-N'-disuccinic acid (HPDDS) are also suitable.
  • Another preferred optional ingredient useful in the composition herein, is one or more additional enzymes.
  • Preferred additional enzymatic materials include the commercially available lipases, cutinases, amylases, neutral and alkaline proteases, esterases, cellulases, pectinases, lactases and peroxidases conventionally incorporated into compositions. Suitable enzymes are discussed in US Patents 3,519,570 and 3,533,139 .
  • protease enzymes include those sold under the tradenames Alcalase, Savinase, Primase, Durazym, and Esperase by Novo Industries A/S (Denmark), those sold under the tradename Maxatase, Maxacal and Maxapem by Gist-Brocades, those sold by Genencor International, and those sold under the tradename Opticlean and Optimase by Solvay Enzymes.
  • Protease enzyme may be incorporated into the composition herein at a level of from 0.0001 % to 4% active enzyme by weight of the composition.
  • Preferred amylases include, for example, ⁇ -amylases obtained from a special strain of B licheniformis, described in more detail in GB-1,269,839 (Novo).
  • Preferred commercially available amylases include for example, those sold under the tradename Rapidase by Gist-Brocades, and those sold under the tradename Termamyl and BAN by Novo Industries A/S.
  • Amylase enzyme may be incorporated into the composition herein at a level of from 0.0001% to 2% active enzyme by weight of the composition.
  • Lipolytic enzyme may be present at levels of active lipolytic enzyme of from 0.0001 % to 10% by weight of the particle, preferably 0.001% to 3% by weight of the composition, most preferably from 0.001 % to 0.5% by weight of the compositions.
  • the lipase may be fungal or bacterial in origin being obtained, for example, from a lipase producing strain of Humicola sp., Thermomyces sp. or Pseudomonas sp. including Pseudomonas pseudoalcaligenes or Pseudomas fluorescens . Lipase from chemically or genetically modified mutants of these strains are also useful herein.
  • a preferred lipase is derived from Pseudomonas pseudoalcaligenes , which is described in Granted European Patent, EP-B-0218272 .
  • Another preferred lipase herein is obtained by cloning the gene from Humicola lanuginosa and expressing the gene in Aspergillus oryza , as host, as described in European Patent Application, EP-A-0258 068 , which is commercially available from Novo Industri A/S, Bagsvaerd, Denmark, under the trade name Lipolase.
  • This lipase is also described in US Patent 4,810,414, Huge-Jensen et al, issued March 7, 1989 .
  • the composition may comprise a suds suppresser at a level less than 10%, preferably 0.001% to 10%, preferably from 0.01% to 8%, most preferably from 0.05% to 5%, by weight of the composition
  • a suds suppresser is either a soap, paraffin, wax, or any combination thereof. If the suds suppresser is a suds suppressing silicone, then the detergent composition preferably comprises from 0.005% to 0.5% by weight a suds suppressing silicone.
  • Suitable suds suppressing systems for use herein may comprise essentially any known antifoam compound, including, for example silicone antifoam compounds and 2-alkyl alcanol antifoam compounds.
  • antifoam compound any compound or mixtures of compounds which act such as to depress the foaming or sudsing produced by a solution of the composition herein, particularly in the presence of agitation of that solution.
  • Particularly preferred antifoam compounds for use herein are silicone antifoam compounds defined herein as any antifoam compound including a silicone component. Such silicone antifoam compounds also typically contain a silica component.
  • silicone antifoam compounds encompasses a variety of relatively high molecular weight polymers containing siloxane units and hydrocarbyl group of various types.
  • Preferred silicone antifoam compounds are the siloxanes, particularly the polydimethylsiloxanes having trimethylsilyl end blocking units.
  • the composition herein comprises from 0.005% to 0.5% by weight suds suppressing silicone.
  • Suitable antifoam compounds include the monocarboxylic fatty acids and soluble salts thereof. These materials are described in US Patent 2,954,347, issued September 27, 1960 to Wayne St. John .
  • the monocarboxylic fatty acids, and salts thereof, for use as suds suppresser typically have hydrocarbyl chains of 10 to 24 carbon atoms, preferably 12 to 18 carbon atoms.
  • Suitable salts include the alkali metal salts such as sodium, potassium, and lithium salts, and ammonium and alkanolammonium salts.
  • Suitable antifoam compounds include, for example, high molecular weight fatty esters (e.g. fatty acid triglycerides), fatty acid esters of monovalent alcohols, aliphatic C 18 -C 40 ketones (e.g. stearone) N-alkylated amino triazines such as tri- to hexa-alkylmelamines or di- to tetra alkyldiamine chlortriazines formed as products of cyanuric chloride with two or three moles of a primary or secondary amine containing 1 to 24 carbon atoms, propylene oxide, bis stearic acid amide and monostearyl di-alkali metal (e.g. sodium, potassium, lithium) phosphates and phosphate esters.
  • high molecular weight fatty esters e.g. fatty acid triglycerides
  • fatty acid esters of monovalent alcohols e.g. fatty acid esters of monovalent alcohols
  • a preferred suds suppressing system in particular for inclusion in the solid component comprises:
  • a highly preferred particulate suds suppressing system is described in EP-A-0210731 and comprises a silicone antifoam compound and an organic carrier material having a melting point in the range 50°C to 85°C, wherein the organic carrier material comprises a monoester of glycerol and a fatty acid having a carbon chain containing from 12 to 20 carbon atoms.
  • EP-A-0210721 discloses other preferred particulate suds suppressing systems wherein the organic carrier material is a fatty acid or alcohol having a carbon chain containing from 12 to 20 carbon atoms, or a mixture thereof, with a melting point of from 45°C to 80°C.
  • composition herein may also comprise from 0.01% to 10 %, preferably from 0.05% to 0.5% by weight of polymeric dye transfer inhibiting agents.
  • polymeric dye transfer inhibiting agents are in addition to the polymeric material of the water-soluble film.
  • the polymeric dye transfer inhibiting agents are preferably selected from polyamine N-oxide polymers, copolymers of N-vinylpyrrolidone and N-vinylimidazole, polyvinylpyrrolidonepolymers or combinations thereof.
  • Polyamine N-oxide polymers suitable for use herein contain units having the following structure formula : wherein P is a polymerisable unit, and R are aliphatic, ethoxylated aliphatics, aromatic, heterocyclic or alicyclic groups or any combination thereof whereto the nitrogen of the N-O group can be attached or wherein the nitrogen of the N-O group is part of these groups.
  • the N-O group can be represented by the following general structures : wherein R1, R2, and R3 are aliphatic groups, aromatic, heterocyclic or alicyclic groups or combinations thereof, x or/and y or/and z is 0 or 1 and wherein the nitrogen of the N-O group can be attached or wherein the nitrogen of the N-O group forms part of these groups.
  • the N-O group can be part of the polymerisable unit (P) or can be attached to the polymeric backbone or a combination of both.
  • Suitable polyamine N-oxides wherein the N-O group forms part of the polymerisable unit comprise polyamine N-oxides wherein R is selected from aliphatic, aromatic, alicyclic or heterocyclic groups.
  • R is selected from aliphatic, aromatic, alicyclic or heterocyclic groups.
  • One class of said polyamine N-oxides comprises the group of polyamine N-oxides wherein the nitrogen of the N-O group forms part of the R-group.
  • Preferred polyamine N-oxides are those wherein R is a heterocyclic group such as pyrridine, pyrrole, imidazole, pyrrolidine, piperidine, quinoline, acridine and derivatives thereof.
  • polyamine N-oxides are the polyamine oxides whereto the N-O group is attached to the polymerisable unit.
  • a preferred class of these polyamine N-oxides comprises the polyamine N-oxides having the general formula (I) wherein R is an aromatic, heterocyclic or alicyclic groups wherein the nitrogen of the N-O functional group is part of said R group.
  • R is an aromatic, heterocyclic or alicyclic groups wherein the nitrogen of the N-O functional group is part of said R group.
  • examples of these classes are polyamine oxides wherein R is a heterocyclic compound such as pyrridine, pyrrole, imidazole and derivatives thereof.
  • the polyamine N-oxides can be obtained in almost any degree of polymerization.
  • the degree of polymerization is not critical provided the material has the desired water-solubility and dye-suspending power.
  • the average molecular weight is within the range of 500 to 1000,000.
  • Suitable herein are co-polymers of N-vinylimidazole and N-vinylpyrrolidone having an average molecular weight range of from 5,000 to 50,000.
  • the preferred copolymers have a molar ratio of N-vinylimidazole to N-vinylpyrrolidone from 1 to 0.2.
  • composition herein may also utilize polyvinylpyrrolidone ("PVP") having an average molecular weight of from 2,500 to 400,000.
  • PVP polyvinylpyrrolidone
  • Suitable polyvinylpyrrolidones are commercially available from ISP Corporation, New York, NY and Montreal, Canada under the product names PVP K-15 (viscosity molecular weight of 10,000), PVP K-30 (average molecular weight of 40,000), PVP K-60 (average molecular weight of 160,000), and PVP K-90 (average molecular weight of 360,000).
  • PVP K-15 is also available from ISP Corporation.
  • Other suitable polyvinylpyrrolidones which are commercially available from BASF Co-operation include Sokalan HP 165 and Sokalan HP 12.
  • composition herein may also utilize polyvinyloxazolidones as polymeric dye transfer inhibiting agents.
  • Said polyvinyloxazolidones have an average molecular weight of from 2.500 to 400,000.
  • composition herein may also utilize polyvinylimidazole as polymeric dye transfer inhibiting agent.
  • Said polyvinylimidazoles preferably have an average molecular weight of from 2,500 to 400,000.
  • composition herein may also optionally comprise from 0.005% to 5% by weight of certain types of hydrophilic optical brighteners.
  • Hydrophilic optical brighteners useful herein include those having the structural formula: wherein R 1 is selected from anilino, N-2-bis-hydroxyethyl and NH-2-hydroxyethyl; R 2 is selected from N-2-bis-hydroxyethyl, N-2-hydroxyethyl-N-methylamino, morphilino, chloro and amino; and M is a salt-forming cation such as sodium or potassium.
  • R 1 is anilino
  • R 2 is N-2-bis-hydroxyethyl and M is a cation such as sodium
  • the brightener is 4,4',-bis[(4-anilino-6-(N-2-bis-hydroxyethyl)-s-triazine-2-yl)amino]-2,2'-stilbenedisulfonic acid and disodium salt.
  • This particular brightener species is commercially marketed under the tradename Tinopal-UNPA-GX by Ciba-Geigy Corporation. Tinopal-UNPA-GX is the preferred hydrophilic optical brightener useful in the compositions herein.
  • R 1 is anilino
  • R 2 is N-2-hydroxyethyl-N-2-methylamino
  • M is a cation such as sodium
  • the brightener is 4,4'-bis[(4-anilino-6-(N-2-hydroxyethyl-N-methylamino)-s-triazine-2-yl)amino]2,2'-stilbenedisulfonic acid disodium salt.
  • This particular brightener species is commercially marketed under the tradename Tinopal 5BM-GX by Ciba-Geigy Corporation.
  • R 1 is anilino
  • R 2 is morphilino
  • M is a cation such as sodium
  • the brightener is 4,4'-bis[(4-anilino-6-morphilino-s-triazine-2-yl)amino]2,2'-stilbenedisulfonic acid, sodium salt.
  • This particular brightener species is commercially marketed under the tradename Tinopal AMS-GX by Ciba Geigy Corporation.
  • compositions herein include perfumes, colours and filler salts, with sodium sulphate being a preferred filler salt.
  • the multi-compartment pouch dissolves or disintegrates in water to deliver the solid detergent ingredients and liquid detergent ingredients to the washing cycle.
  • the multi-compartment pouch is added to the dispensing draw, or alternatively to the drum, of an automatic washing machine.
  • the multi-compartment pouch comprises all of the detergent ingredients of the detergent composition used in the washing. Although it may be preferred that some detergent ingredients are not comprised by the multi-compartment pouch and are added to the washing cycle separately.
  • one or more detergent compositions other than the detergent composition comprised by the multi-compartment pouch can be used during the laundering process, such that said detergent composition comprised by the multi-compartment pouch is used as a pre-treatment, main-treatment, post-treatment or a combination thereof during such a laundering process.
  • a piece of plastic is placed in a mould to act as a false bottom.
  • the mould consists of a cylindrical shape and has a diameter of 45mm and a depth of 25mm.
  • a 1mm thick layer of rubber is present around the edges of the mould.
  • the mould has some holes in the mould material to allow a vacuum to be applied. With the false bottom in place the depth of the mould is 12mem.
  • a piece of Chris-Craft M-8630 film is placed on top of this mould and fixed in place. A vacuum is applied to pull the film into the mould and pull the film flush with the inner surface of the mould and the false bottom. 5ml of the liquid component of a detergent composition is poured into the mould.
  • a second piece of Chris-Craft M-8630 film is placed over the top of the mould with the liquid component and sealed to the first piece of film by applying an annular piece of flat metal of an inner diameter of 46mm and heating that metal under moderate pressure onto the ring of rubber at the edge of the mould to heat-seal the two pieces of film together to form a compartment comprising the liquid component.
  • the metal ring is typically heated to a temperature of from 135°C to 150°C and applied for up to 5 seconds.
  • the compartment comprising the liquid compartment is removed from the mould and the piece of plastic acting as a false bottom is also removed from the mould.
  • a third piece of Chris-Craft M-8630 film is placed on top of the mould and fixed in place.
  • a vacuum is applied to pull the film into the mould and pull the film flush with the inner surface of the mould. 40g of the solid component of the detergent composition is poured into the mould.
  • the compartment comprising the liquid component is placed over the top of the mould with the solid component and is sealed to the third layer of film by applying an annular piece of flat metal of an inner diameter of 46mm and heating that metal under moderate pressure onto the ring of rubber at the edge of the mould to heat-seal the pieces of film together to form a pouch comprising two compartments, where a first compartment comprises the liquid component of the detergent composition and a second compartment comprises the solid component of the detergent composition.
  • the metal ring is typically heated to a temperature of from 135°C to 150°C and applied for up to 5 seconds.
  • a pouch was made by the process described in example I which comprises the following liquid component and solid component.
  • Solid component detergent ingredient Amount (by weight of the Solid component) Zeolite 40% Surfactant 11 % Bleach 20% Chelating agent 0.8% Enzyme 6% Suds suppressor 1% Bleach activator 12% Sodium carbonate 6% Soap 1% Brightener 0.5% Minors to 100%
  • Liquid component detergent ingredient Amount (by weight of liquid component)
  • a pouch was made by the process described in example I which comprises the following liquid component and solid component.
  • Solid component detergent ingredient Amount (by weight of the solid component) Zeolite 64% Bleach 16% Chelating agent 2% Enzyme 10% Suds suppressor 1% Sodium carbonate 4% Brightener 1% Minors to 100%
  • Liquid component detergent ingredient Amount (by weight of liquid component)
  • Nonionic surfactant 69% Solvent 179% Perfume 10% Water 3% Minors to 100%

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Packages (AREA)
  • Bag Frames (AREA)
  • Wrappers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Claims (4)

  1. Sachet à compartiments multiples constitué d'un film hydrosoluble comprenant un polymère d'alcool polyvinylique et ayant au moins deux compartiments, ledit sachet à compartiments multiples comprend une composition comprenant un composant solide et un composant liquide, dans lequel ;
    (a) un premier compartiment comprend un composant solide comprenant (en poids du composant solide) au moins 10 % de matériau solide insoluble dans l'eau qui est un agent d'adjuvance insoluble dans l'eau qui est un aluminosilicate ou un agent d'adoucissement des tissus insoluble dans l'eau qui est de l'argile ; et
    (b) un deuxième compartiment comprend un composant liquide.
  2. Sachet à compartiments multiples selon l'une quelconque des revendications précédentes, dans lequel ledit composant solide comprend (en poids du composant solide) au moins 50 % de matériau insoluble dans l'eau.
  3. Sachet à compartiments multiples selon l'une quelconque des revendications précédentes, dans lequel ledit composant solide comprend, en outre, au moins un élément choisi dans le groupe constitué d'un agent chélatant, une source de peroxyde d'hydrogène, un activateur de blanchiment, une enzyme, un azurant et un suppresseur de mousse.
  4. Sachet à compartiments multiples selon l'une quelconque des revendications précédentes, dans lequel ledit composant liquide comprend au moins deux éléments choisis dans le groupe constitué d'un agent tensioactif non ionique, un parfum, un acide gras ou un sel de celui-ci, et un solvant.
EP01916548A 2000-04-28 2001-03-09 Compositions en sachet Expired - Lifetime EP1276843B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB0010227 2000-04-28
GB0010227A GB2361707A (en) 2000-04-28 2000-04-28 Pouched compositions
PCT/US2001/007707 WO2001083657A2 (fr) 2000-04-28 2001-03-09 Compositions en sachet

Publications (2)

Publication Number Publication Date
EP1276843A2 EP1276843A2 (fr) 2003-01-22
EP1276843B1 true EP1276843B1 (fr) 2009-10-28

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EP (1) EP1276843B1 (fr)
JP (1) JP5490344B2 (fr)
KR (1) KR100500755B1 (fr)
CN (1) CN1225538C (fr)
AR (1) AR033353A1 (fr)
AT (1) ATE447004T1 (fr)
AU (1) AU2001243561A1 (fr)
BR (1) BR0110256A (fr)
CA (1) CA2404657C (fr)
DE (1) DE60140298D1 (fr)
ES (1) ES2333516T3 (fr)
GB (1) GB2361707A (fr)
MX (1) MXPA02010581A (fr)
WO (1) WO2001083657A2 (fr)

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US7125828B2 (en) 2000-11-27 2006-10-24 The Procter & Gamble Company Detergent products, methods and manufacture
US8283300B2 (en) 2000-11-27 2012-10-09 The Procter & Gamble Company Detergent products, methods and manufacture
JP4107387B2 (ja) * 2001-11-14 2008-06-25 ザ プロクター アンド ギャンブル カンパニー スケール形成防止ポリマーを含む１回用量の形態の自動食器洗浄用組成物
DE102004030148B4 (de) * 2004-06-22 2007-10-31 Henkel Kgaa Verfahren zur Herstellung von Portionspackungen für wasch- oder reinigungsaktive Substanzen
DE102004030318B4 (de) 2004-06-23 2009-04-02 Henkel Ag & Co. Kgaa Mehrkammer-Pouch
DE102004051619A1 (de) 2004-10-22 2006-04-27 Henkel Kgaa Wasch- oder Reinigungsmittel
DE102004062328A1 (de) * 2004-12-20 2006-06-29 Henkel Kgaa Dosiereinheit für Wasch- oder Reinigungsmittel
MX2007009952A (es) 2005-02-17 2007-09-26 Procter & Gamble Composicion para el cuidado de telas.
DE102005025690B4 (de) * 2005-04-27 2007-02-01 Henkel Kgaa Verpackungssystem für Wasch-oder Reinigungsmittel
DE102005020009A1 (de) * 2005-04-27 2006-11-09 Henkel Kgaa Wasch- oder Reinigungsmittel Dosiereinheit
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EP2011856B1 (fr) * 2007-07-02 2011-11-23 The Procter & Gamble Company Procédé de traitement du linge
US8097047B2 (en) 2008-04-02 2012-01-17 The Procter & Gamble Company Fabric color rejuvenation composition
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EP2333039B2 (fr) † 2009-12-10 2020-11-11 The Procter & Gamble Company Procédé et utilisation d'une composition pour lave-vaisselle
EP2333040B2 (fr) † 2009-12-10 2019-11-13 The Procter & Gamble Company Composition de détergent
BR112013000101A2 (pt) 2010-07-02 2016-05-17 Procter & Gamble filamentos compreendendo mantas de não tecido com agente ativo e métodos de fabricação dos mesmos
CA2803636C (fr) 2010-07-02 2017-05-16 The Procter & Gamble Company Produit detergent et son procede de fabrication
MX2012015187A (es) 2010-07-02 2013-05-09 Procter & Gamble Metodo para suministrar un agente activo.
EP2857485A1 (fr) 2013-10-07 2015-04-08 WeylChem Switzerland AG Poche à compartiments multiples comprenant des compositions de nettoyage sans alkanolamine, processus de lavage et utilisation de produits de lavage et de nettoyage de textiles et plats
HUE035129T2 (en) 2014-02-27 2018-05-02 Unilever Nv Water-soluble detergent capsule with reduced fine fine particles in HEDP
CN103923775A (zh) * 2014-04-08 2014-07-16 余姚市德派日用品有限公司 一种家用洗衣洗碗包
EP3207085B1 (fr) * 2014-10-13 2021-07-21 Monosol, LLC Film à base de polyvinyle et d'alcool soluble dans l'eau, procédés associés et articles associés
CN104403849A (zh) * 2014-10-28 2015-03-11 江南大学 一种水溶膜包装的固体洗涤剂组合物
CN105886169B (zh) * 2014-12-15 2019-09-13 上海和黄白猫有限公司 粉状洗涤剂包及其制备方法
CN104974864A (zh) * 2015-07-23 2015-10-14 广州柏俐臣化妆品有限公司 一种多功能洗衣凝珠及其制备方法
CN107384654B (zh) * 2016-05-17 2021-04-27 北京绿伞化学股份有限公司 一种除垢去污防护产品
TW201815636A (zh) * 2016-10-18 2018-05-01 雨宮克治 包裝體
TW201815635A (zh) * 2016-10-18 2018-05-01 雨宮克治 包裝體
CN110167639B (zh) 2017-01-27 2022-10-14 宝洁公司 呈包含泡腾型附聚颗粒的可溶性固体结构形式的组合物
EP3624765A1 (fr) 2017-05-16 2020-03-25 The Procter and Gamble Company Compositions de conditionnement pour soins capillaires sous la forme de structures solides solubles
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JP2003531781A (ja) 2003-10-28
DE60140298D1 (de) 2009-12-10
GB2361707A (en) 2001-10-31
MXPA02010581A (es) 2003-03-10
CN1426454A (zh) 2003-06-25
BR0110256A (pt) 2003-01-07
KR20020086962A (ko) 2002-11-20
CN1225538C (zh) 2005-11-02
JP5490344B2 (ja) 2014-05-14
ES2333516T3 (es) 2010-02-23
AU2001243561A1 (en) 2001-11-12
CA2404657C (fr) 2007-07-24
GB0010227D0 (en) 2000-06-14
AR033353A1 (es) 2003-12-17
WO2001083657A2 (fr) 2001-11-08
CA2404657A1 (fr) 2001-11-08
WO2001083657A3 (fr) 2002-01-31
EP1276843A2 (fr) 2003-01-22
KR100500755B1 (ko) 2005-07-12
ATE447004T1 (de) 2009-11-15

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