WO2001085898A1 - Detergent product - Google Patents
Detergent product Download PDFInfo
- Publication number
- WO2001085898A1 WO2001085898A1 PCT/US2001/007710 US0107710W WO0185898A1 WO 2001085898 A1 WO2001085898 A1 WO 2001085898A1 US 0107710 W US0107710 W US 0107710W WO 0185898 A1 WO0185898 A1 WO 0185898A1
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- WO
- WIPO (PCT)
- Prior art keywords
- compartment
- pouch
- composition
- water
- seal
- Prior art date
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Classifications
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B11/00—Wrapping, e.g. partially or wholly enclosing, articles or quantities of material, in strips, sheets or blanks, of flexible material
- B65B11/50—Enclosing articles, or quantities of material, by disposing contents between two sheets, e.g. pocketed sheets, and securing their opposed free margins
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- 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
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- 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
Definitions
- This invention relates to water-soluble pouches.
- Incompatible detergent ingredients are comprised by different compartments of said pouch in such a manner so that they do not come into contact with each other until said pouch dissolves or disintegrates in water during the washing cycle.
- the inventors have found that there is a risk of detergent ingredients leaking from multi- compartment pouches, in addition the inventors have found that detergent ingredients are more likely to leak from the seals of a multi-compartment pouch, especially when the compartments are sealed simultaneously, due to the poor seal strength. The risk of leakage is greater when one of the compartments comprises a liquid.
- the inventors have found that if the compartments are sealed simultaneously, a process which requires unsealed compartments being in relatively close proximity, there is a risk that ingredients may leak from one unsealed compartment to another during the sealing process, due the lack of a seal to prevent the exchange of ingredients between the two compartments during the early stages of the sealing process. This is especially applicable if one or more of the ingredients is a liquid.
- the inventors have found that by using a pre-sealed water-soluble compartment to close an unsealed compartment, thus forming a multi-compartment water-soluble pouch, said multi-compartment water-soluble pouch is more stable having a reduced risk of ingredients leaking from the seals of said pouch both during the manufacturing and storage of the pouch. This is due to the multiple seal that is formed by the above closing process. This is especially applicable if the pre-sealed water-soluble compartment comprises a liquid.
- a multi-compartment pouch made from a water- soluble film and having at least two compartments, said multi-compartment pouch is obtainable by the process of closing an open compartment with a pre-sealed compartment, the process forms a second seal on the pre-sealed compartment which is in a different position to the first seal of the pre-sealed compartment.
- a process for making a multi-compartment pouch made from a water-soluble film and having at least two compartments comprises the step of closing an open compartment with a pre-sealed compartment.
- the multi-compartment pouch herein referred to as "pouch" has at least two, preferably two compartments.
- the pouch herein is typically a closed structure, made of materials described herein, enclosing a volume space which preferably comprises a composition. Said composition is described in more detail herein.
- the pouch 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 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 compartment of the pouch is a closed structure, made of materials described herein, enclosing a volume space which comprises the components. 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.
- 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".
- the term "outside environment” means for the purpose of this invention "anything which cannot pass through the water-soluble film which encloses the compartment and which is not comprised by the compartment".
- the volume space of the open compartment is greater than the volume space of the pre-sealed compartment.
- the compartment of the pouch which is derived from the open compartment has a volume space which is greater than the compartment of the pouch which is derived from the pre-sealed compartment.
- the pouch preferably comprises a composition, said composition may comprise a solid component or a liquid component. If the composition comprises a solid component and a liquid component, then it may be preferred that the solid component and liquid component are comprised by two different compartments, typically so that that said solid component and said liquid component are separated by a water-soluble film which acts as a barrier.
- a compartment which comprises a 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 the compartment.
- the presence of the air bubble increases the tolerance of the pouch to the movement of liquid ingredients within the compartments of the pouch, thus reducing the risk of liquid ingredients leaking from the pouch.
- the compartment is suitable to hold the components, 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 composition is a composition to be delivered to water and thus the pouch and the compartment(s) thereof are designed such that at least one or more of the components is released at or very shortly after the time of addition to the water. It is especially preferred that at least one component is delivered to the water within 3 minutes, preferably even within 2 minutes or even within 1 minute after contacting the pouch to water.
- the compartment and preferably the pouch as a whole comprises material which is water-dispersible or more preferably water-soluble.
- Preferred water-dispersible material herein has a dispersability 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.
- the material is water-soluble and 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 pouch is made from a water-soluble film.
- Preferred films are polymeric materials, preferably polymers which are formed into a film or sheet.
- the film can for example be obtained by casting, blow-moulding, extrusion or blow extrusion of the polymer material, as known in the art.
- Preferred polymer copolymers or derivatives thereof are selected from polyvinyl alcohols, polyvinyl pyrrolidone, polyalkylene oxides, acrylamide, acrylic acid, cellulose, cellulose ethers, cellulose esters, cellulose amides, polyvinyl acetates, polycarboxylic acids and salts, polyaminoacids or peptides, polyamides, polyacrylamide, copolymers of maleic/acrylic acids, polysaccharides including starch and gelatine, natural gums such as xanthum and carragum.
- the polymer is selected from polyacrylates and water-soluble acrylate copolymers, methylcellulose, carboxymethylcellulose sodium, dextrin, ethylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose, maltodextrin, polymethacrylates, most preferably polyvinyl alcohols, polyvinyl alcohol co-polymers, polyvinyl alcohol ter-polymers, and hydroxypropyl methyl cellulose (HPMC).
- polyacrylates and water-soluble acrylate copolymers methylcellulose, carboxymethylcellulose sodium, dextrin, ethylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose, maltodextrin, polymethacrylates, most preferably polyvinyl alcohols, polyvinyl alcohol co-polymers, polyvinyl alcohol ter-polymers, and hydroxypropyl methyl cellulose (HPMC).
- the polymer can have any weight average molecular weight, preferably from about 1000 to 1,000,000, or even form 10,000 to 300,000 or even form 15,000 to 200,000 or even form 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% to 98% hydrolysed, preferably 80% to 90%, to improve the dissolution of the material.
- Suitable examples of commercially available water-soluble films include polyvinyl alcohol and partially hydrolysed polyvinyl acetate, alginates, cellulose ethers such as carboxymethylcellulose and methylcellulose, polyethylene oxide, polyacrylates and combinations thereof. Most preferred are films which comprises PVA polymers and have similar properties to films that are 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 pouched composition is a detergent composition, that the pouch or compartment material itself comprises a detergent additive to be delivered to the wash water, for example organic polymeric soil release agents, dispersants, dye transfer inhibitors.
- the pouch is obtainable by the process of closing an open compartment with a pre-sealed compartment.
- Said process comprises the step of closing an open compartment with a pre-sealed compartment.
- Said process forms a second seal in a different position to the first seal of the pre-sealed compartment.
- said second seal has a greater equivalent surface diameter than the first seal of the pre-sealed compartment.
- An open compartment has a volume space that is not separated from the outside environment.
- the process of closing the open compartment forms a compartment that has a volume space which is separated from the outside environment, such a compartment is a closed compartment, such as a compartment of the multi-compartment pouch of the invention.
- the open compartment can be done by any known method.
- the open compartment is formed by fitting a water-soluble pouch around a mould and vacuum pulling the film so that it is flush with the inner surface of the mould, thus forming a volume space which is not separated from the outside environment, said volume space being the vacuum formed indent or niche in said water-soluble film.
- Preferred open compartments are made by introducing the film to form the compartment to a mould, then applying a vacuum to the mould, so that the material adopts the shape of the mould, also referred to as vacuum-forming.
- Another preferred method is thermo- forming to get the material to adopt the shape of the mould.
- the process of closing typically comprises the steps of;
- a mould is used in the process for producing the pouch, especially if a mould is used in the process step of closing the open compartment with a pre-sealed compartment, then preferably the pre-sealed compartment is formed in a different mould to the mould used to close the open compartment with the pre-sealed compartment.
- the open compartment is closed with the same material as the material of the open compartment.
- the closing material and thus preferably also the open compartment material, is preferably thermoplastic so that it can be closed by heat-sealing.
- a thermoplastic coating may be provided, either over the whole material or just in the areas where seals are to be formed.
- the sealing can also be made by solvent welding.
- Suitable heat-sealable materials include polyvinyl alcohol, polyvinyl acetate, polyvinyl pyrrolidone, polyethylene oxide, acrylic resins and mixtures thereof, in particular polyvinyl alcohols (PVA). These heat-sealable materials may also be used in combination with the other water-soluble or water-dispersible materials.
- the pre-sealed compartment is typically already sealed prior to contact to the open compartment in such a manner so that any ingredient comprised in the volume space of the pre-sealed compartment is separated from the outside environment.
- the pre-sealed compartment typically comprises at least one seal, preferably only one seal, prior to the process of closing the open compartment.
- the seal formed by the process of closing has a greater equivalent surface diameter than the seal already present on the pre-sealed compartment.
- greater equivalent surface diameter it is typically meant that the diameter of the second seal is longer than the diameter of the first seal.
- the seal formed by the process of closing closes the open compartment, adds a second seal to the pre-sealed compartment, and forms a multi-compartment pouch by structurally bringing together the open compartment and pre-sealed compartment to form a multi-compartment pouch.
- the pouch preferably comprises a composition, typically said composition is contained in the volume space of the compartments of the pouch.
- the composition 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 comprises at least one surfactant and at least one building agent.
- the composition may comprises a solid component and a liquid component.
- the pre-sealed compartment comprises a liquid component. Said liquid component and solid component are described in more detail herein.
- the liquid component is comprised by a compartment of the pouch.
- said compartment is a different compartment to the compartment that comprises the solid component.
- liquid component includes components in the form of a viscous liquid and or a gel.
- the liquid component preferably comprises (by weight of the liquid component) at least 50%, preferably at least 55%, more preferably at least 60%, more preferably at least 70%, more preferably at least 80% surfactant.
- the surfactant is a liquid at room temperature.
- the surfactant is a nonionic surfactant, an anionic surfactant or a combination thereof, most preferably the surfactant is a nonionic surfactant.
- said liquid component of the invention comprises a solvent or a perfume.
- said liquid component comprises (by weight of the liquid component) at least 2%, more preferably at least 5%, more preferably at least 10%, more preferably at least 40% perfume.
- 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.
- said solvent is an alcohol based solvent, more preferably said solvent is ethanol and/or n-butoxy propoxy propanol.
- 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 solid component is comprised by a compartment of the pouch.
- said compartment is a different compartment to the compartment that comprises the liquid component.
- Said solid component preferably comprises (by weight of the solid component) at least 10%, more preferably at least 20%, more preferably at least 30% water-insoluble solid material.
- said water-insoluble solid material includes water-insoluble building agents, preferably the water-insoluble building agent is an aluminosilicate, or water-insoluble fabric softening agent such as clay.
- said water-insoluble solid material comprises a water-insoluble building agent. Preferred water-insoluble building agents are described in more detail hereinafter.
- Said solid composition preferably comprises at least one detergent ingredient selected from the group consisting of building agent, chelating agent, bleaching agent, bleach activator, enzyme, brightener, suds suppressor and dye.
- said detergent ingredient is in the form of a solid.
- 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.
- the composition herein typically comprises ingredients. These ingredients are described hereinafter.
- the composition may comprises a liquid component and a solid component.
- ingredients that are preferably manufactured and processed in a solid form are comprised by the solid component and ingredients that are preferably manufactured and processed in a liquid form are comprised by the liquid component.
- the preferred amounts of ingredients described herein are % by weight of the composition herein as a whole and not % by weight of either the solid component or liquid component which may comprise said ingredient.
- the composition herein preferably comprises a water-insoluble building agent.
- the water-insoluble building agent is comprised by the solid component.
- the water-insoluble building agent is in solid form.
- water insoluble builders include the sodium aluminosilicates.
- the aluminosilicate material may be 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.
- Chelating agents The composition herein, preferably comprises a chelating agent.
- heavy chelating agent 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.
- Chelating agents 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 chelating agents 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.
- any alkoxylated nonionic surfactants can be comprised by the composition herein.
- the ethoxylated and propoxylated nonionic surfactants are preferred.
- Preferred alkoxylated surfactants can be selected from the classes of the nonionic 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 herein.
- a highly preferred nonionic polyhydroxy fatty acid amide surfactant for use herein is a C12-C14 , a C ⁇ 5-C17 and/or C ⁇ g-Ci g alkyl N-methyl glucamide. It may be particularly preferred that the composition herein comprises a mixture of a C12-
- Fatty acid amide surfactants or alkoxylated fatty acid amides can also be comprised by the composition herein.
- Alkyl esters of fatty acids can also be comprised by the composition herein.
- Alkylpolysaccharides can also be comprised by the composition herein, such as those 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.
- 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 friethanolamine salts) of the anionic sulphate, sulphonate, carboxylate and sarcosinate surfactants. Anionic sulphate surfactants are preferred.
- 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 C5-C17 acyl-N-(C ⁇ -C4 alkyl) and -N-(C ⁇ -C2 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 C9-C22 alkyl sulphates, more preferably the C1 1 -C15 branched chain alkyl sulphates and the C12-C14 linear chain alkyl sulphates.
- Anionic sulphonate surfactants suitable for use herein include the salts of C5-C20 linear or branched alkylbenzene sulphonates, alkyl ester sulphonates, in particular methyl ester sulphonates, Cg-C22 primary or secondary alkane sulphonates, C6-C24 olefin sulphonates, sulphonated polycarboxylic acids, alkyl glycerol sulphonates, fatty acyl glycerol sulphonates, fatty oleyl glycerol sulphonates, and any mixtures thereof.
- Suitable anionic surfactants are the alkali metal sarcosinates.
- Preferred examples are the myristyl and oleoyl methyl sarcosinates in the form of their sodium salts.
- Cationic surfactant 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 of the composition herein.
- the ratio of the anionic surfactant to the cationic surfactant is preferably from 35:1 to 1:3, more preferably from 15:1 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.
- Suitable amphoteric surfactants for use herein include the amine oxide surfactants and the alkyl amphocarboxylic acids.
- Preferred amine oxides are C10-C1 g alkyl dimethylamine oxide, and C10-I8 acylamido alkyl dimethylamine oxide.
- a suitable example of an alkyl aphodicarboxylic acid is Miranol(TM) C2M Cone, 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. Complex betaine surfactants are also suitable for use herein.
- the composition herein may comprises 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.
- 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.
- 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 polymerisation 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.
- 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. Preferably 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.
- Alkali metal percarbonates, particularly sodium percarbonate are preferred perhydrates herein.
- Sodium percarbonate is an addition compound having a formula corresponding to 2Na2CO3.3H2O2, 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.
- 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.
- Amide substituted alkyl peroxyacid precursor compounds are also suitable for use herein.
- the organic peroxyacid bleaching system may contain a pre-formed organic peroxyacid.
- Preferred organic peroxyacids include 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.
- 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.
- protease enzymes include those sold under the tradenames Alcalase, Savinase, Primase, Durazym, and Esperase by Novo Industries A/S (Denmark), those sold under the fradename Maxatase, Maxacal and Maxapem by Gist- Brocades, those sold by Genencor International, and those sold under the fradename 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.
- 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, preferred lipase is commercially available from Novo Industri A S, Bagsvaerd, Denmark, under the trade name Lipolase.
- 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
- the 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.
- Particularly preferred suds suppressers are silicone antifoam compounds defined herein as any antifoam compound including a silicone component.
- Preferred silicone antifoam compounds are the siloxanes, particularly the polydimethylsiloxanes having frimethylsilyl end blocking units.
- Other suitable antifoam compounds include the monocarboxylic fatty acids and soluble salts thereof.
- 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 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, polyvmylpyrrolidonepolymers or combinations thereof.
- a preferred optical brightener is 4,4',-bis[(4-anilino-6-(N-2-bis-hydroxyethyl)-s-triazine- 2-yl)amino]-2,2'-stilbenedisulfonic acid and disodium salt, which is 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.
- Another preferred brightener is 4,4'-bis[(4-anilino-6-(N-2-hydroxyethyl-N-methylamino)-s- friazine-2-yl)amino]2,2'-stilbenedisulfonic acid disodium salt, which is commercially marketed under the tradename Tinopal 5BM-GX by Ciba-Geigy Corporation. Also, 4,4'- bis[(4-anilino-6-morphilino-s-triazine-2-yl)amino]2,2'-stilbenedisulfonic acid, sodium salt, is a preferred optical brightener and is marketed under the tradename Tinopal AMS- GX by Ciba Geigy Corporation.
- Cationic fabric softening agents are preferably present in the composition herein.
- Suitable cationic fabric softening agents include the water insoluble tertiary amines or dilong chain amide materials.
- these water-insoluble tertiary amines or dilong chain amide materials are comprised by the solid component of the composition herein.
- Cationic fabric softening agents are typically incorporated at total levels of from 0.5% to 15% by weight, normally from 1% to 5% by weight.
- 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-freatment, main-freatment, post-treatment or a combination thereof during such a laundering process.
- a piece of Chris-Craft M-8630 film is placed on top of a small mould and fixed in place.
- the small mould consists of a hemispherical shape and has a diameter of 33mm and a depth of 14.5mm.
- 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 A vacuum is applied to pull the film into the mould and pull the film flush with the inner surface of the mould. 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 small 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 34mm 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 pre-sealed compartment comprismg the liquid component.
- the metal ring is typically heated to a temperature of froml35°C to 150°C and applied for up to 5 seconds.
- the pre-sealed compartment has a 75mm rim of Chris-Craft film which extends in an outwardly direction from the seal away from the centre of the pre-sealed compartment so that the pre-sealed compartment can be fixed into place and completely cover the opening of a mould with a larger diameter of 48.5mm.
- a third piece of Chris-Craft M-8630 film is placed on top of a larger mould and fixed in place.
- the large mould consists of a cylindrical shape and has a diameter of 48.5mm and a depth of 22mm. 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 A vacuum is applied to pull the film into the large mould and pull the film flush with the inner surface of the mould to form an open compartment. 40g of the solid component of the detergent composition is poured into the open compartment.
- the rim of film of the pre-sealed compartment is sealed to the third layer of film by applying an annular piece of flat metal of an inner diameter of 50mm 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 froml35°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.
- Liquid component detergent ingredient Amount (by weight of the liquid component)
- Solid component detergent ingredient Amount (by weight of the solid component)
- a pouch was made by the process described in example I which comprises the following liquid component and solid component.
- Liquid component detergent ingredient Amount (by weight of liquid component)
Landscapes
- 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)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Detergent Compositions (AREA)
- Packages (AREA)
- Bag Frames (AREA)
- Woven Fabrics (AREA)
Abstract
Description
Claims
Priority Applications (10)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP01916551A EP1276844B1 (en) | 2000-04-28 | 2001-03-09 | Detergent product |
BR0110269-9A BR0110269A (en) | 2000-04-28 | 2001-03-09 | Detergent product |
AT01916551T ATE269398T1 (en) | 2000-04-28 | 2001-03-09 | LAUNDRY DETERGENT |
CA002404678A CA2404678C (en) | 2000-04-28 | 2001-03-09 | Multi-compartment pouch made with pre-sealed compartment |
JP2001582488A JP2003532599A (en) | 2000-04-28 | 2001-03-09 | Detergent products |
AU2001243564A AU2001243564A1 (en) | 2000-04-28 | 2001-03-09 | Detergent product |
MXPA02010582A MXPA02010582A (en) | 2000-04-28 | 2001-03-09 | Detergent product. |
DE60103883T DE60103883T2 (en) | 2000-04-28 | 2001-03-09 | LAUNDRY DETERGENT |
US10/278,239 US7022659B2 (en) | 2000-04-27 | 2002-10-23 | Packaged unit dose of detergent and method of treating fabrics |
US10/279,589 US6995126B2 (en) | 2000-04-28 | 2002-10-24 | Pouched compositions |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB0010229A GB2361686A (en) | 2000-04-28 | 2000-04-28 | Water-soluble, multi-compartment pouch for detergent product |
GB0010229.3 | 2000-04-28 |
Related Child Applications (3)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2001/013456 Continuation WO2001081530A1 (en) | 2000-04-27 | 2001-04-25 | Packaging for unit dose of detergent and method of its use |
US10/278,239 Continuation US7022659B2 (en) | 2000-04-27 | 2002-10-23 | Packaged unit dose of detergent and method of treating fabrics |
US10/279,589 Continuation US6995126B2 (en) | 2000-04-28 | 2002-10-24 | Pouched compositions |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2001085898A1 true WO2001085898A1 (en) | 2001-11-15 |
Family
ID=9890587
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2001/007710 WO2001085898A1 (en) | 2000-04-27 | 2001-03-09 | Detergent product |
Country Status (12)
Country | Link |
---|---|
EP (1) | EP1276844B1 (en) |
JP (1) | JP2003532599A (en) |
CN (1) | CN1426455A (en) |
AT (1) | ATE269398T1 (en) |
AU (1) | AU2001243564A1 (en) |
BR (1) | BR0110269A (en) |
CA (1) | CA2404678C (en) |
DE (1) | DE60103883T2 (en) |
ES (1) | ES2222986T3 (en) |
GB (1) | GB2361686A (en) |
MX (1) | MXPA02010582A (en) |
WO (1) | WO2001085898A1 (en) |
Cited By (17)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6956016B2 (en) | 2001-05-14 | 2005-10-18 | The Procter & Gamble Company | Cleaning product |
WO2006000309A1 (en) * | 2004-06-23 | 2006-01-05 | Henkel Kommanditgesellschaft Auf Aktien | Multi-chambered pouch |
WO2006088980A1 (en) | 2005-02-17 | 2006-08-24 | The Procter & Gamble Company | Fabric care composition |
EP1790713A2 (en) | 2000-11-27 | 2007-05-30 | The Procter & Gamble Company | Detergent products, methods and manufacture |
WO2008000567A1 (en) * | 2006-06-30 | 2008-01-03 | Unilever Plc | Laundry articles |
US7429273B2 (en) | 2002-10-12 | 2008-09-30 | Reckitt Benckiser N.V. | Carpet cleaning composition |
EP2011856A1 (en) * | 2007-07-02 | 2009-01-07 | The Procter and Gamble Company | Method of treating laundry |
US7507698B2 (en) | 2002-02-27 | 2009-03-24 | Reckitt Benckiser N.V. | Textile articles for washing and cleaning applications |
WO2011011247A1 (en) | 2009-07-20 | 2011-01-27 | The Procter & Gamble Company | Liquid fabric enhancer composition comprising a di-hydrocarbyl complex |
US7891515B2 (en) | 2002-08-07 | 2011-02-22 | Reckitt Benckiser (Uk) Limited | Water soluble container with rigid spacer |
US8097047B2 (en) | 2008-04-02 | 2012-01-17 | The Procter & Gamble Company | Fabric color rejuvenation composition |
US8367599B2 (en) * | 2001-03-16 | 2013-02-05 | Unilever Home & Personal Care Usa, Division Of Conopco, Inc. | Dishwashing composition with particles |
US8669219B2 (en) | 2007-01-18 | 2014-03-11 | Reckitt Benckiser N.V. | Dosage element and a method of manufacturing a dosage element |
US8754025B2 (en) | 2007-01-18 | 2014-06-17 | Reckitt Benckiser N.V. | Dosage element and a method of manufacturing a dosage element |
US8980817B2 (en) | 2007-01-18 | 2015-03-17 | Reckitt Benckiser N.V. | Dosage element and a method of manufacturing a dosage element |
US9868926B2 (en) | 2007-01-18 | 2018-01-16 | Reckitt Benckiser Finish B.V. | Dosage element and a method of manufacturing a dosage element |
US11225348B2 (en) | 2015-05-22 | 2022-01-18 | The Procter & Gamble Company | Process of making a water soluble pouch |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8658585B2 (en) | 2000-11-27 | 2014-02-25 | Tanguy Marie Louise Alexandre Catlin | Detergent products, methods and manufacture |
US7125828B2 (en) | 2000-11-27 | 2006-10-24 | The Procter & Gamble Company | Detergent products, methods and manufacture |
US20020137648A1 (en) | 2000-11-27 | 2002-09-26 | Sanjeev Sharma | Dishwashing method |
US6624130B2 (en) | 2000-12-28 | 2003-09-23 | Unilever Home & Personal Care Usa Division Of Conopco, Inc. | Laundry product |
EP1666579B2 (en) * | 2004-11-22 | 2012-11-28 | The Procter & Gamble Company | Water-soluble, liquid-containing pouch |
CN103320244A (en) * | 2013-07-04 | 2013-09-25 | 余姚市德派日用品有限公司 | Environment-friendly household clothes/dish washing bag |
EP2924102A1 (en) * | 2014-03-24 | 2015-09-30 | The Procter and Gamble Company | Laundry unit dose article |
CN103923775A (en) * | 2014-04-08 | 2014-07-16 | 余姚市德派日用品有限公司 | Household clothes-washing and dish-washing bag |
EP4159418A1 (en) * | 2021-10-01 | 2023-04-05 | The Procter & Gamble Company | Process of sealing water-soluble polyvinylalcohol films |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4973416A (en) * | 1988-10-14 | 1990-11-27 | The Procter & Gamble Company | Liquid laundry detergent in water-soluble package |
WO1993008091A2 (en) * | 1991-10-16 | 1993-04-29 | Rhone-Poulenc Agriculture Ltd. | Sealed package |
US5224601A (en) * | 1990-07-18 | 1993-07-06 | Rhone-Poulenc Ag Company | Water soluble package |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NZ244818A (en) * | 1991-10-24 | 1994-09-27 | Rhone Poulenc Agrochimie | Package containing a toxic composition which comprises two compartments formed by two sheets of water-soluble dispersible material by means of a water-soluble/dispersible heat seal and a third sheet |
-
2000
- 2000-04-28 GB GB0010229A patent/GB2361686A/en not_active Withdrawn
-
2001
- 2001-03-09 JP JP2001582488A patent/JP2003532599A/en not_active Withdrawn
- 2001-03-09 WO PCT/US2001/007710 patent/WO2001085898A1/en active IP Right Grant
- 2001-03-09 CA CA002404678A patent/CA2404678C/en not_active Expired - Fee Related
- 2001-03-09 ES ES01916551T patent/ES2222986T3/en not_active Expired - Lifetime
- 2001-03-09 AU AU2001243564A patent/AU2001243564A1/en not_active Abandoned
- 2001-03-09 CN CN01808713.2A patent/CN1426455A/en active Pending
- 2001-03-09 AT AT01916551T patent/ATE269398T1/en not_active IP Right Cessation
- 2001-03-09 DE DE60103883T patent/DE60103883T2/en not_active Expired - Lifetime
- 2001-03-09 MX MXPA02010582A patent/MXPA02010582A/en unknown
- 2001-03-09 BR BR0110269-9A patent/BR0110269A/en not_active IP Right Cessation
- 2001-03-09 EP EP01916551A patent/EP1276844B1/en not_active Expired - Lifetime
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4973416A (en) * | 1988-10-14 | 1990-11-27 | The Procter & Gamble Company | Liquid laundry detergent in water-soluble package |
US5224601A (en) * | 1990-07-18 | 1993-07-06 | Rhone-Poulenc Ag Company | Water soluble package |
WO1993008091A2 (en) * | 1991-10-16 | 1993-04-29 | Rhone-Poulenc Agriculture Ltd. | Sealed package |
Cited By (24)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1790713A2 (en) | 2000-11-27 | 2007-05-30 | The Procter & Gamble Company | Detergent products, methods and manufacture |
EP1790713A3 (en) * | 2000-11-27 | 2007-09-05 | The Procter & Gamble Company | Detergent products, methods and manufacture |
EP1337619B2 (en) † | 2000-11-27 | 2013-06-19 | The Procter & Gamble Company | Detergent methods |
US8367599B2 (en) * | 2001-03-16 | 2013-02-05 | Unilever Home & Personal Care Usa, Division Of Conopco, Inc. | Dishwashing composition with particles |
US7078462B2 (en) | 2001-05-14 | 2006-07-18 | The Procter & Gamble Company | Cleaning product |
US6956016B2 (en) | 2001-05-14 | 2005-10-18 | The Procter & Gamble Company | Cleaning product |
US7507698B2 (en) | 2002-02-27 | 2009-03-24 | Reckitt Benckiser N.V. | Textile articles for washing and cleaning applications |
US7891515B2 (en) | 2002-08-07 | 2011-02-22 | Reckitt Benckiser (Uk) Limited | Water soluble container with rigid spacer |
US7429273B2 (en) | 2002-10-12 | 2008-09-30 | Reckitt Benckiser N.V. | Carpet cleaning composition |
WO2006000309A1 (en) * | 2004-06-23 | 2006-01-05 | Henkel Kommanditgesellschaft Auf Aktien | Multi-chambered pouch |
US7446084B2 (en) | 2004-06-23 | 2008-11-04 | Henkel Kommanditgesellschaft Auf Aktien | Process for manufacturing multi-phase detergents or cleaning agents in a water-soluble container |
WO2006088980A1 (en) | 2005-02-17 | 2006-08-24 | The Procter & Gamble Company | Fabric care composition |
WO2008000567A1 (en) * | 2006-06-30 | 2008-01-03 | Unilever Plc | Laundry articles |
US7977298B2 (en) | 2006-06-30 | 2011-07-12 | The Sun Products Corporation | Laundry articles |
US8669219B2 (en) | 2007-01-18 | 2014-03-11 | Reckitt Benckiser N.V. | Dosage element and a method of manufacturing a dosage element |
US8754025B2 (en) | 2007-01-18 | 2014-06-17 | Reckitt Benckiser N.V. | Dosage element and a method of manufacturing a dosage element |
US8980817B2 (en) | 2007-01-18 | 2015-03-17 | Reckitt Benckiser N.V. | Dosage element and a method of manufacturing a dosage element |
US9868926B2 (en) | 2007-01-18 | 2018-01-16 | Reckitt Benckiser Finish B.V. | Dosage element and a method of manufacturing a dosage element |
US9902926B2 (en) | 2007-01-18 | 2018-02-27 | Reckitt Benckiser Finish B.V. | Dosage element and a method of manufacturing a dosage element |
US10294446B2 (en) | 2007-01-18 | 2019-05-21 | Reckitt Benckiser Finish B.V. | Dosage element and a method of manufacturing a dosage element |
EP2011856A1 (en) * | 2007-07-02 | 2009-01-07 | The Procter and Gamble Company | Method of treating laundry |
US8097047B2 (en) | 2008-04-02 | 2012-01-17 | The Procter & Gamble Company | Fabric color rejuvenation composition |
WO2011011247A1 (en) | 2009-07-20 | 2011-01-27 | The Procter & Gamble Company | Liquid fabric enhancer composition comprising a di-hydrocarbyl complex |
US11225348B2 (en) | 2015-05-22 | 2022-01-18 | The Procter & Gamble Company | Process of making a water soluble pouch |
Also Published As
Publication number | Publication date |
---|---|
CN1426455A (en) | 2003-06-25 |
CA2404678C (en) | 2007-04-24 |
DE60103883D1 (en) | 2004-07-22 |
EP1276844A1 (en) | 2003-01-22 |
ES2222986T3 (en) | 2005-02-16 |
MXPA02010582A (en) | 2003-03-10 |
DE60103883T2 (en) | 2005-07-07 |
GB2361686A (en) | 2001-10-31 |
GB0010229D0 (en) | 2000-06-14 |
AU2001243564A1 (en) | 2001-11-20 |
EP1276844B1 (en) | 2004-06-16 |
CA2404678A1 (en) | 2001-11-15 |
JP2003532599A (en) | 2003-11-05 |
ATE269398T1 (en) | 2004-07-15 |
BR0110269A (en) | 2003-02-18 |
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