US20110191965A1 - Method of cleaning an object - Google Patents
Method of cleaning an object Download PDFInfo
- Publication number
- US20110191965A1 US20110191965A1 US13/120,238 US200913120238A US2011191965A1 US 20110191965 A1 US20110191965 A1 US 20110191965A1 US 200913120238 A US200913120238 A US 200913120238A US 2011191965 A1 US2011191965 A1 US 2011191965A1
- Authority
- US
- United States
- Prior art keywords
- foam composition
- enzyme
- pressure
- wash
- container
- 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.)
- Abandoned
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- HXITXNWTGFUOAU-UHFFFAOYSA-N phenylboronic acid Chemical class OB(O)C1=CC=CC=C1 HXITXNWTGFUOAU-UHFFFAOYSA-N 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-M phosphonate Chemical compound [O-]P(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-M 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920002006 poly(N-vinylimidazole) polymer Polymers 0.000 description 1
- 229920000196 poly(lauryl methacrylate) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920005996 polystyrene-poly(ethylene-butylene)-polystyrene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- RYMZZMVNJRMUDD-HGQWONQESA-N simvastatin Chemical compound C([C@H]1[C@@H](C)C=CC2=C[C@H](C)C[C@@H]([C@H]12)OC(=O)C(C)(C)CC)C[C@@H]1C[C@@H](O)CC(=O)O1 RYMZZMVNJRMUDD-HGQWONQESA-N 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- HSFQBFMEWSTNOW-UHFFFAOYSA-N sodium;carbanide Chemical group [CH3-].[Na+] HSFQBFMEWSTNOW-UHFFFAOYSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 125000001273 sulfonato group Chemical group [O-]S(*)(=O)=O 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 239000001226 triphosphate Substances 0.000 description 1
- 235000011178 triphosphate Nutrition 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- 239000012588 trypsin Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—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
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0052—Gas evolving or heat producing compositions
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06F—LAUNDERING, DRYING, IRONING, PRESSING OR FOLDING TEXTILE ARTICLES
- D06F35/00—Washing machines, apparatus, or methods not otherwise provided for
- D06F35/005—Methods for washing, rinsing or spin-drying
- D06F35/006—Methods for washing, rinsing or spin-drying for washing or rinsing only
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06F—LAUNDERING, DRYING, IRONING, PRESSING OR FOLDING TEXTILE ARTICLES
- D06F39/00—Details of washing machines not specific to a single type of machines covered by groups D06F9/00 - D06F27/00
- D06F39/02—Devices for adding soap or other washing 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
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/12—Soft surfaces, e.g. textile
-
- 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
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
Definitions
- the present invention relates to the field of cleaning.
- the invention relates to methods of cleaning an object employing alternating pressure.
- Laundering is in general performed by agitating the fabrics in a detergent solution for a certain period of time followed by rinsing the fabrics in water. Laundering may be carried out using an automatic washing machine or it may be done by hand.
- Modern detergents are complex compositions comprising a number of components such as; surfactants, builders, bleaches, polymers, enzymes etc. just to mention a few, and are usually formulated as a powder or a liquid.
- EP0086935 describes a method of washing soiled textile goods where foam is created and blown on the textile. The benefit of the method is that it can be performed using small amounts of detergent and water.
- GB2340846 describes a method of washing items comprising; placing items in a vessel, introducing a washing liquid thereto, reducing pressure within the vessel and thereby causing gas/vapor to bubble through the liquid. The purpose of reducing the pressure is to create bubbling of gas/vapor to agitate the items as an alternative to mechanical agitation. The reduction in pressure is furthermore used to cause boiling of the washing liquid thereby avoiding that items being exposed to temperatures needed to boil said liquid at atmospheric pressure.
- EP0677577 describes a method of cleaning textiles by using foam whereby the foam or foam residues on the textiles subsequently being substantially removed by application of vacuum.
- EP0765932 describes a method of cleaning and conditioning textile fabrics by applying foam comprising a fabric softening clay and subsequently removing foam residues by vacuum.
- the invention in a first aspect relates to a method for cleaning an object comprising the steps: (a) placing the object to be cleaned in an alternating pressure resistant container; (b) applying to the object a foam composition comprising at least one foaming agent, at least one enzyme and a dissolved gas; (c) cleaning the object with the foam composition by applying alternating pressure to the container; and (d) rinsing the object.
- the invention in a second aspect relates to a method for rinsing an object comprising the steps: (a) placing the object to be rinsed in an alternating pressure resistant container; (b) applying to the object a rinse liquid; (c) rinsing the object with the rinse liquid by applying alternating pressure to the container.
- FIG. 1 shows wash performance of WAP compared to beaker wash and a standard fine wash.
- FIG. 2 shows wash performance of WAP compared to wash at constant pressure.
- FIG. 3 shows the effect of WAP rinse compared to that of beaker rinse on wash performance.
- FIG. 4 shows the effect of WAP rinse compared to that of beaker rinse on the amount of residual LAS in the rinse solution.
- FIG. 5 shows a schematic drawing of a WAP device.
- FIG. 6 shows a picture of the WAP device used.
- AP The tem “AP” as used herein means alternating pressure.
- WAP The terms “WAP” or “WAP wash” as used herein means washing with alternating pressure.
- WAP rinse means rinsing with alternating pressure.
- wash performance means the delta remission measured at 440 nm of the swatch, where delta remission is the remission measured at 440 nm of a washed swatch minus the remission measured at 440 nm of an unwashed swatch.
- Plateau border means the transition zone formed when bubbles/films meet. Except for free-floating bubbles, films have to be supported by frames, bulk surfaces or other films. The transition zone separating these from the film proper, always containing some bulk liquid, is called a plateau border.
- the soiled textile is immersed in a detergent solution and subjected to mechanical action, followed by repeated rinsing with water, and drying.
- the detergent solution generally includes surfactants and enzymes.
- the detergent is typically formulated with a view to avoid foaming.
- the invention is based on the observation that when an enzyme enriched foam are added to the fabric/textile and micro-mechanical action is applied by means of alternating pressure surprisingly increased wash performance is obtained compared to conventional wash. Alternating pressure may furthermore be utilized during rinsing whereby an improved rinsing is obtained.
- Water consumption is reduced for washing as well as for rinsing because the alternating pressure principles may be used to speed up the dilution and exchange of wash active ingredients and soil to the suds and the rinse water.
- the invention may furthermore result in reduced energy and resource consumption compared to that of conventional washing processes because the macro-mechanical action (turning the drum) is avoided, and heating can either be eliminated or reduced due to the combined action of enzyme and alternating pressure.
- the invention relates to a method for cleaning an object comprising the steps: (a) placing the object to be cleaned in an alternating pressure resistant container; (b) applying to the object a foam composition comprising at least one foaming agent, at least one enzyme and a dissolved gas; (c) cleaning the object with the foam composition by applying alternating pressure to the container; and (d) rinsing the object.
- the foam composition comprises at least one foaming agent, at least one enzyme and a dissolved gas. It is typically an aqueous foam composition. It is preferred that the foam composition is particular adapted to use in the method according to the invention.
- the at least one foaming agent may in principle be any such known foaming agent capable of forming stable foam, such as high foaming surfactants selected among: non-ionic surfactants; anionic surfactants; cationic surfactants; ampholytic surfactants; zwitterionic surfactants; semi-polar surfactants; or any combinations thereof.
- the kind and concentration of surfactants may be chosen with a view to good foam formation and compatibility with the at least one enzyme.
- the surfactants are typically present at a level of from 0.1% to 60% by weight; from 0.1% to 30%; from 0.1% to 20%; from 0.1% to 10%; from 0.1% to 5%; from 0.1% to 1% by weight.
- the foam composition will usually contain from about 0.1% to about 40%; from 0.1% to 30%; from 0.1% to 20%; from 0.1% to 10%; from 0.1% to 5%; from 0.1% to 1% by weight of an anionic surfactant such as linear alkylbenzenesulfonate, alpha-olefinsulfonate, alkyl sulfate (fatty alcohol sulfate), alcohol ethoxysulfate, secondary alkanesulfonate, alpha-sulfo fatty acid methyl ester, alkyl- or alkenylsuccinic acid or soap.
- an anionic surfactant such as linear alkylbenzenesulfonate, alpha-olefinsulfonate, alkyl sulfate (fatty alcohol sulfate), alcohol ethoxysulfate, secondary alkanesulfonate, alpha-sulfo fatty acid methyl ester, alkyl- or alkenylsuccinic acid or soap.
- the foam composition will usually contain from about 0.1% to about 40%; from 0.1% to 30%; from 0.1% to 20%; from 0.1% to 10%; from 0.1% to 5%; from 0.1% to 1% by weight of a non-ionic surfactant such as alcohol ethoxylate, nonylphenol ethoxylate, alkylpolyglycoside, alkyldimethylamineoxide, ethoxylated fatty acid monoethanolamide, fatty acid monoethanolamide, polyhydroxy alkyl fatty acid amide, or N-acyl N-alkyl derivatives of glucosamine (“glucamides”).
- glucamides N-acyl N-alkyl derivatives of glucosamine
- foaming agent is selected among anionic surfactants.
- foaming agents include Eucerin and sodium linear C 12 alkyl benzene sulphonate (LAS).
- the invention relates to a method, wherein the at least one foaming agent is selected from: non-ionic, anionic surfactants; cationic surfactants; ampholytic surfactants; zwitterionic surfactants; semi-polar surfactants; or any combinations thereof.
- the invention relates to a method, wherein the anionic surfactant is selected from: linear alkylbenzene sulfonate; alpha-olefin sulfonate; alkyl sulfonate (fatty alcohol sulfonate); alcohol ethoxy sulfonate; secondary alkane sulfonate; alpha-sulfo fatty acid methyl ester; alkyl- or alkenyl succinic acid or soap, or any combination thereof.
- the anionic surfactant is selected from: linear alkylbenzene sulfonate; alpha-olefin sulfonate; alkyl sulfonate (fatty alcohol sulfonate); alcohol ethoxy sulfonate; secondary alkane sulfonate; alpha-sulfo fatty acid methyl ester; alkyl- or alkenyl succinic acid or soap, or any combination thereof.
- the invention relates to a method, wherein the concentration of the foaming agent is 0.1%-60% w/w relative to the soiled object.
- the at least one enzyme comprised in the foam composition according to some embodiments of the invention may in principle be any enzyme known to have an effect on soiled objects such as fabrics/textiles.
- Such enzymes may e.g. be enzymes traditionally used in laundering, having optimal activity in the neutral to alkaline range, or enzymes having optimal activity in the acidic to neutral range, and may include at least one enzyme selected from the group containing: amylases; arabinases; carbohydrases; cellulases; cutinases; galactanases; haloperoxidases; hydrolases; laccases; lipases; mannanases; oxidases; oxidoreductases; pectinases; peroxidases; proteases; xylanases.
- the at least one enzyme comprised in the foam composition, and accordingly the method according to some embodiments of the invention, are described in further details below:
- Amylase Any amylase ( ⁇ and/or ⁇ ) may in principle be used. Suitable amylases include those of bacterial or fungal origin. Chemically or genetically modified mutants are included. Amylases include, for example, ⁇ -amylases obtained from a special strain of B. licheniformis , described in more detail in GB 1,296,839. Commercially available amylases are DuramylTM, TermamylTM, FungamylTM and BANTM (Novozymes NS) and RapidaseTM and Maxamyl PTM (Genencor).
- Cellulase Any cellulase may in principle be used. Suitable cellulases include those of bacterial or fungal origin. Chemically or genetically modified mutants are included. Suitable cellulases are disclosed in U.S. Pat. No. 4,435,307, which discloses fungal cellulases produced from Humicola insolens . Especially suitable cellulases are the cellulases having colour care benefits. Examples of such cellulases are cellulases described in EP0495257. Commercially available cellulases include CelluzymeTM produced by a strain of Humicola insolens , (Novozymes A/S), and KAC-500(B)TM (Kao Corporation).
- Suitable lipases include those of bacterial or fungal origin. Chemically or genetically modified mutants are included. Examples of useful lipases include a Humicola lanuginosa lipase, e.g., as described in EP 258 068 and EP 305 216, a Rhizomucor miehei lipase, e.g., as described in EP 238 023, a Candida lipase, such as a C. antarctica lipase, e.g., the C. antarctica lipase A or B described in EP 214 761, a Pseudomonas lipase such as a P. alcaligenes and P.
- a Humicola lanuginosa lipase e.g., as described in EP 258 068 and EP 305 216
- Rhizomucor miehei lipase e.g., as described in EP 238 023
- Candida lipase such as a
- pseudoalcaligenes lipase e.g., as described in EP0218272, a P. cepacia lipase, e.g., as described in EP0331376, a P. stutzeri lipase, e.g., as disclosed in GB 1,372,034, a P. fluorescens lipase, a Bacillus lipase, e.g., a B. subtilis lipase (Dartois et al., (1993), Biochemica et Biophysica acta 1131, 253-260), a B. stearothermophilus lipase (JP 64/744992) and a B.
- pumilus lipase (WO 91/16422). Furthermore, a number of cloned lipases may be useful, including the Penicillium camembertii lipase described by Yamaguchi et al. (1991) Gene vol. 103, p. 61-67, the Geotricum candidum lipase (Schimada, Y. et al. (1989) J. Biochem. Vol. 106, p. 383-388), and various Rhizopus lipases such as a R. delemar lipase (Hass, M. J et al. (1991) Gene vol. 109, p. 117-113), a R. niveus lipase (Kugimiya et al. (1992) Biosci. Biotech. Biochem. Vol. 56, p. 716-719) and a R. oryzae lipase.
- Penicillium camembertii lipase described by Yama
- cutinases may also be useful, e.g., a cutinase derived from Pseudomonas mendocina as described in WO 88/09367, or a cutinase derived from Fusarium solani pisi (e.g. described in WO 90/09446).
- lipases such as M1 LipaseTM, Luma fastTM and Lipo-maxTM (Genencor), LipolaseTM and Lipolase UltraTM (Novo Nordisk NS), and Lipase P “Amano” (Amano Pharmaceutical Co. Ltd.).
- Peroxidases/oxidases Peroxidase enzymes are used in combination with hydrogen peroxide or a source thereof (e.g. a percarbonate, perborate or persulfate). Oxidase enzymes are used in combination with oxygen. Both types of enzymes are used for “solution bleaching”, i.e. to prevent transfer of a textile dye from a dyed fabric to another fabric when said fabrics are washed together in a wash liquor, preferably together with an enhancing agent as described in e.g. WO 94/12621 and WO 95/01426. Suitable peroxidases/oxidases include those of plant, bacterial or fungal origin. Chemically or genetically modified mutants are included.
- proteases include those of animal, vegetable or microbial origin. Microbial origin is preferred. Chemically or genetically modified mutants are included.
- the protease may be a serine protease, preferably an alkaline microbial protease or a trypsin-like protease.
- alkaline proteases are subtilisins, especially those derived from Bacillus , e.g., subtilisin Novo, subtilisin Carlsberg, subtilisin 309, subtilisin 147 and subtilisin 168 described in WO 89/06279.
- trypsin-like proteases are trypsin (e.g.
- protease enzymes include those sold under the trade names Alcalase, Savinase, Primase, Durazym, and Esperase (Novozymes A/S), those sold under the tradename Maxatase, Maxacal, Maxapem, Properase, Purafect and Purafect OXP (Genencor) and those sold under the tradename Opticlean and Optimase (Solvay Enzymes).
- Mixtures of the above mentioned enzymes are encompassed herein, in particular a mix-ture of proteases, amylases, lipases and/or cellulases.
- the at least one enzyme, each individual enzyme or the total amount of enzyme may be incorporated into the foam composition in accordance with some embodiments of the invention at a level of from 0.00001% to 30%; from 0.00001% to 20%; from 0.00001% to 10%; from 0.0001% to 5%; from 0.001% to 2%; or from 0.01% to 1% of enzyme by volume of the total foam composition.
- the invention relates to a method, wherein the at least one enzyme is selected from: amylases; arabinases; carbohydrases; cellulases; cutinases; galactanases; haloperoxidases; hydrolases; lipases; mannanases; oxidases e.g. laccases or peroxidases; oxidoreductases; pectinases proteases; xylanases; or any combination thereof.
- the at least one enzyme is selected from: amylases; arabinases; carbohydrases; cellulases; cutinases; galactanases; haloperoxidases; hydrolases; lipases; mannanases; oxidases e.g. laccases or peroxidases; oxidoreductases; pectinases proteases; xylanases; or any combination thereof.
- the invention relates to a method, wherein the concentration of the at least one enzyme is from 0.00001% to 10%; from 0.0001% to 5%; from 0.001% to 2%; or from 0.01% to 1% of enzyme by volume of the total foam composition.
- the foam composition contains dissolved gas, typically atmospheric air. Tap water contains enough atmospheric air and may thus be used directly. Alternatively, degassed water or other liquids may be supplied with any suitable gas and used in the foam composition.
- a suitable gas may e.g. be atmospheric air, carbon dioxide etc. or a mixture of suitable gasses.
- the foam composition may in some embodiments of the invention further comprise at least one other agent selected among: fabric conditioners including clays; anti-corrosion agents; hydrotropes; redeposition agents; foam boosters; foam stabilizing agents; suds suppressors; enzyme stabilizing agents; pH regulating agents; builder systems; bleaching agents; soil-releasing agents; soil suspending agents; polymeric dye transfer inhibiting agents; optical brighteners; abrasives; bactericides; tarnish inhibitors; softening agents; dyes; coloring agents; and perfume, some of which are described below.
- fabric conditioners including clays; anti-corrosion agents; hydrotropes; redeposition agents; foam boosters; foam stabilizing agents; suds suppressors; enzyme stabilizing agents; pH regulating agents; builder systems; bleaching agents; soil-releasing agents; soil suspending agents; polymeric dye transfer inhibiting agents; optical brighteners; abrasives; bactericides; tarnish inhibitors; softening agents; dyes; coloring agents; and perfume, some of
- the foam composition may further comprise one or more foam stabilizers such as glucosides or emulsifiers known to be able of stabilizing water/surfactant/gas emulsions.
- foam stabilizers such as glucosides or emulsifiers known to be able of stabilizing water/surfactant/gas emulsions.
- the foam composition may also contain pH regulating agents known in the art, such as inorganic salts like phosphates, sulphates and carbonates; organic compounds like carboxylic acids, carboxylates, amines, sulphonates etc. pH regulating agents should be selected to provide a pH value of the foam composition which is compatible or preferably optimal for the at least one enzyme included in the foam composition. pH regulating agents according to some embodiments of the invention includes well known buffer components such as glycine and sodium carbonate.
- the foam compositions according to the invention contain no mandatory soap or surfactant components and are therefore not restricted to maintain a pH value in a particular range but the pH value of the compositions can be selected in order to obtain optimal conditions for the enzymes comprised in the composition.
- the pH of the foam composition can be in the acidic range, in the alkaline range or it can be neutral.
- the pH can be selected in the range of 4-10, more preferred in the range of 5-9.
- the foam composition has an acidic pH value i.e. pH below 7 such as pH in the range of 4-7 and the enzymes are selected in order to have maximal activity under acidic conditions
- a neutral pH value i.e. pH about 7 and the enzymes are selected in order to have maximal activity under neutral conditions
- in a third embodiment has the foam composition an alkaline pH value i.e. pH above 7 such as pH in the range of 7-10 and the enzymes are selected in order to have maximal activity under alkaline conditions.
- the foam composition may contain 0-65% by weight of a builder or complexing agent such as zeolite, diphosphate, triphosphate, phosphonate, carbonate, citrate, nitrilotriacetic acid, ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, alkyl- or alkenylsuccinic acid, soluble silicates or layered silicates (e.g. SKS-6 from Hoechst).
- a builder or complexing agent such as zeolite, diphosphate, triphosphate, phosphonate, carbonate, citrate, nitrilotriacetic acid, ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, alkyl- or alkenylsuccinic acid, soluble silicates or layered silicates (e.g. SKS-6 from Hoechst).
- Enzyme stabilizers The at least one enzyme comprised in the foam composition of the invention may be stabilized using conventional stabilizing agents, e.g., a polyol such as propylene glycol or glycerol, a sugar or sugar alcohol, lactic acid, boric acid, or a boric acid derivative, e.g., an aromatic borate ester, or a phenyl boronic acid derivative such as 4-formylphenyl boronic acid.
- a polyol such as propylene glycol or glycerol
- a sugar or sugar alcohol lactic acid, boric acid, or a boric acid derivative, e.g., an aromatic borate ester, or a phenyl boronic acid derivative such as 4-formylphenyl boronic acid.
- the foam composition may in some embodiments of the invention comprise one or more polymers.
- Examples are carboxymethylcellulose, poly(vinylpyrrolidone), poly(ethylene glycol), poly(vinyl alcohol), poly(vinylpyridine-N-oxide), poly(vinylimidazole), polycarboxylates such as polyacrylates, maleic/acrylic acid copolymers and lauryl methacrylate/acrylic acid copolymers.
- the foam composition may in some embodiments of the invention contain a bleaching system which may comprise a H 2 O 2 source such as perborate or percarbonate which may be combined with a peracid-forming bleach activator such as tetraacetylethylenediamine or nonanoyloxybenzenesulfonate.
- a bleaching system may comprise peroxyacids of e.g. the amide, imide, or sulfone type.
- the foam compositions of the invention may in principle be made using known foaming methods. Methods for preparing foam are well known within the area of cleaning hard surfaces in e.g. the food industry, and it should be understood that such well known methods and equipment used for such methods may also be applied to the present invention.
- One method for preparing the foam composition according to the invention is mixing and foaming the ingredients in a high shear mixer.
- Another method for preparing the foam composition according to the invention is providing the ingredients under pressure in a container together with a suitable propellant and creating the foam composition by dispensing the composition through a suitable orifice using technologies as will be well know from spray cans or aerosol cans.
- the propellant may be any compound that is a compressible gas at ambient temperature and is inert toward the foam compositions; however it is preferred to use a propellant that is harmless for the users and the environment.
- propellants as will be well known in the art may also be used within the present invention.
- suitable propellants are e.g. nitrogen, propane and butane.
- Another method for making foam is to use the conventional method for foam dispersion in e.g. hard surface cleaning, by having a concentrated surfactant in a container.
- a water flow draws out a suitable amount of surfactant (to the water) to a foaming nozzle.
- the concentration of surfactant is dependent on the water pressure.
- the enzyme may be included in the container together with the surfactant or it can be placed in a separate container and drawn out into the water flow before or after the surfactant to the foaming nozzle. Alternatively, all components of the foam composition is added together before it enters the alternating pressure resistant container through the foam nozzle.
- the foam composition manually, by mixing the ingredients and foaming of the mixture using mechanical action, e.g. by whipping the foam or by using a hand foamer.
- Hand foamers are known in the art and may also be applicable in some embodiments of the present invention.
- the foam composition When the foam composition is applied to the object it is important that it is evenly distributed in order to secure best possible conditions for cleaning.
- Application, distribution and/or re-distribution of the foam composition may be obtained by mixing, agitating, shaking, ultrasound or any combination thereof. It may be done by hand; using a stick, spatula, or the like; or it may be performed using a suitable device.
- the foam composition may alternatively be applied through the inlet and the inlet nozzle of the alternating pressure resistant container of the invention.
- Distribute or redistribution of the foam composition evenly to the object in the container may be done by ways as indicated above for a short period of time like e.g. 0.5; 1.0; 1.5; 2.0; 2.5; 3.0; 3.5; 4.0; 4.5; or 5.0 minutes until the foam composition is evenly distributed.
- the object to be cleaned may be any fabrics, textile, laundry, leather, skin, fur or hard surfaces.
- the invention relates to a method, wherein the object is: fabrics; textiles; laundry; leather; skin; fur; or hard surfaces.
- a “hydrodynamic barrier” is formed. This barrier which is about 1 micrometer in thickness is generated by water molecules which through polar hydrogen bonds are packed like a film upon the surface of the object to be cleaned. Depending of the hydrophobic or hydrophilic nature of the object said barrier may act more or less efficiently as a barrier and interfere in the exchange of molecules between the foam composition and the surface of the object.
- Washing in a front loader machine applies mechanical action by letting the textile load drop from the top of the drum to the bottom in the presence of a wash solution.
- This macro-mechanical action breaks parts of the hydrodynamic barrier thereby promoting interaction between wash solution and textile.
- a traditional wash foam is undesirable because it acts as an insulator.
- the foam may act as an extra hydrodynamic barrier on the object thereby increasing the thickness of the barrier considerably, thereby preventing removal of soil from the textile during washing and during rinsing.
- alternating pressure generates mechanical action on a microscopically level within the hydrodynamic barrier.
- the wash liqueur is added as a foam composition which is absorbed by the fabric/textile and in particular porous materials may contain relatively large amounts of foam.
- the pressure is lowered the dissolved gas present in the foam composition will appear as bubbles which increase in size.
- Dependent on the viscoelasiticity of the foam composition changes in bubble size creates micro-mechanical action both within as well as at the surface of the fabric/textile. This action promotes exchange of active components from the foam composition to textile fibres and transport released soil and decomposition products away from the textile.
- the washing step comprises at least one cycle of alternating pressure wherein the pressure in turns is reduced and increased.
- One cycle of alternating pressure correspond to reduced pressure followed by increased pressure.
- a time period wherein alternating pressure is performed may be indicated. During this time period one or more cycles of alternating pressures may take place.
- the dissolved gas comprised in the foam composition forms bubbles and/or enlarges existing bubbles, whereas during increased pressure the bubbles are diminished and/or may partly collapse or dissolve.
- the number of cycles of alternating pressure may vary and accordingly it may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, or 30 cycles.
- the time period of alternating pressure may vary and accordingly it may last 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, or 30 minutes.
- the invention relates to a method, wherein the alternating pressure is at least ⁇ 1.0 bar, at least ⁇ 0.9 bar, at least ⁇ 0.8 bar, at least ⁇ 0.7 bar, at least ⁇ 0.6 bar, at least ⁇ 0.5 bar, at least ⁇ 0.4 bar, at least ⁇ 0.3 bar, at least ⁇ 0.2 bar, at least ⁇ 0.1 bar, or at least 0.1 bar; at least 0.2 bar; at least 0.3 bar, at least 0.4 bar, at least 0.5 bar, at least 0.6 bar, at least 0.7 bar, at least 0.8 bar, at least 0.9 bar, at least 1.0 bar, at least 1.1 bar, at least 1.2 bar, at least 1.3 bar, at least 1.4 bar, at least 1.5 bar, at least 2.0 bar, at least 2.5 bar, at least 3.0 bar, at least 3.5 bar, at least 4.0 bar, at least 4.5 bar, or at least 5.0 bar.
- alternating pressure may be interrupted by recirculation or flushing, wherein the spent foam composition may be drained off and reapplied, or fresh foam composition may be added respectively.
- Recirculation or flushing may serve to remove soiling and/or to replenish dissolved gas.
- Recycling or flushing creates a macro-mechanical action which may be combined with the micro-mechanical action created by alternating pressure.
- This is done by applying said foam composition through the inlet vessel and nozzle of the container. Due to the low pressure the foam composition will enter the container as foam.
- By subsequently applying pressure to the chamber and briefly open an outlet vessel in the bottom of the container the foam composition will be forced through the fabric/textile placed in the container whereby wetting of the object and distribution of the foam composition are obtained.
- This procedure may be used for initial wetting and distribution as well as for recycling or flushing of the foam composition between periods of alternating pressure.
- By recirculation the foam composition will be revitalized for a subsequent period of alternating pressure. And the flow of foam composition also promotes the transport of chemicals as well as substances into the liquid.
- recirculation or flushing foam is created which demands a relatively higher or lower pressure to remove.
- the number of recirculation or flushing should therefore be selected to suit the foam composition for the purpose of creating sufficient foam for cleaning.
- alternating pressure more efficiently helps in controlling and removing foam as compared to conventional rinsing care should be taken to balance the amount of foam.
- the invention relates to a method, wherein the foam composition is redistributed on the object during step (b) and/or after step (c).
- the invention relates to a method, wherein redistribution of the foam composition is obtained by mixing, agitating, shaking, ultra sound, or any combination thereof.
- the invention relates to a method, wherein the foam composition is recycled at least once during cleaning of the object in step (c) by withdrawing said composition through an outlet of the container and reapplying it through an inlet of the container.
- the invention relates to a method, wherein the foam composition is flushed at least once during cleaning of the object in step (c) by withdrawing said composition through an outlet of the container and applying new foam composition through an inlet of the container.
- the invention relates to a method, wherein recycling and/or flushing is performed 2; 3; 4; 5; 6; 7; 8; 9; or 10 times.
- a very important advantage by the method of the invention is foam control. This means that antifoaming agents are not needed to the same extent as they are used in conventional washing solutions today.
- rinsing After washing of an object rinsing may be performed as a conventional rinsing such as rinsing by hand or in a washing machine. Rinsing may also be performed using alternating pressure, WAP rinse where water or another suitable rinse liquid enters the container during low pressure and is squeezed out of the container during high pressure. WAP rinsing may be performed in a similar manner as the washing step by at least one cycle of pressure reduction and increase. The number of cycles of alternating pressure comprised in the WAP rinse may vary and accordingly it may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29 or 30 cycles.
- the time period of alternating pressure may vary and accordingly it may last 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29 or 30 minutes. Between the cycles or the time periods of alternating pressure, spent liquid may be drained off and fresh water/rinse liquid may be added.
- the invention relates to a method, wherein rinsing is obtained by applying to the object a rinse liquid and applying alternating pressure to the container.
- the invention relates to a method for rinsing an object comprising the steps: (a) placing the object to be rinsed in an alternating pressure resistant container; (b) applying to the object a rinse liquid; (c) rinsing the object with the rinse liquid by applying alternating pressure to the container.
- a drying step wherein drying is obtained by applying high or low pressure, heating, centrifugation, or any combination thereof.
- the temperature during cleaning according to the method is not critical as long as the enzymes remain active during said temperature.
- the skilled person will appreciate that some enzymes will be suitable for a low temperature, whereas others may be suitable for higher temperatures. Thus, taking due care to the selection of enzymes and the particular fabrics being laundered a suitable temperature may be selected.
- the temperature is in the range of 0-90° C., 5-50° C., 10-40° C., 15-30° C., 20-25° C.
- the temperature may be an ambient temperature selected among: 20° C., 21° C., 22° C., 23° C., 24° C., or 25° C.
- the present invention offers a tremendous versatility in the laundering process depending of the particular selected foam composition and detergent composition and the particular selection of enzymes included in these compositions.
- a device was specially designed for carrying out the method of the invention.
- the device and operating instructions are described below.
- the text chamber is made of PVC and will tolerate most types of soap as well as strong alkali and acid.
- Chemicals used as buffers and substrates were commercial products of at least reagent grade.
- a fine wash program at 40° C. with a main wash at 30 min+rinse time on a Miele household washing machine was used as a standard wash.
- 65 g Ariel Sensitive (P&G) from Denmark 2008 containing approximately 0.4% protease and 0.2% amylase was used to wash a stain set as indicated in the example and up till 2.6 kg fabric of 5 pillowcases (100% Polyester), 2 close cloth T-shirts (100% Cotton), 5 T-shirts (100% Cotton), 4 shirts (60% Polyester and 40% Cotton) and 1 t-towel (100% Cotton).
- Beaker wash was carried out in a 1000 ml glass beaker. The washing was performed at room temperature (20-22° C.) at pH 9.0 for 30 minutes.
- WAP wash was carried out in a specially designed WAP-equipment based on a alternating pressure resistant container with access to compressed air as described.
- the washing was performed at room temperature (20-22° C.) at pH 9.0 for 30 minutes followed by rinsing.
- the low pressure manometer is put on 0.5 bar and the pressure manometer is put on 0.45 bar.
- Delta remission was measured at 440 nm using a Macbeth Color-Eye 7000 (Largo AB, Box 5259, refstg ⁇ rdstempen 3, SE-402 25 Göteborg, Sweden). The washed swatches were placed on a grid, covered with paper, and left over night at room temperature to dry. Next day delta remission of the swatches were determined.
- Redeposition was tested by adding the tracer swatches Wfk10A (100% cotton, Prewashed) and Wfk30A (100% polyester, prewashed) together with soiled swatches and ballast fabric during washing and rinsing.
- the tracer swatches were placed on a grid, covered with paper, and left over night at room temperature to dry. Next day delta remission at 440 nm of the tracer swatches were determined.
- wash performance indicated on the y-axis is the sum accumulated from the delta remission for all the individual swatches tested in the same wash. Delta remission values for individual swatches as well as the sum are listed in the tables.
- the wash performance is illustrated in FIG. 1 showing that WAP wash (column 4) results in a better wash performance in comparison with beaker wash when using identical foam compositions (enzyme rich LAS foam). This result is independent of whether there is no agitation (column 1) or brief agitation for 1.5 min (column 2) or agitation for 9 min (column 3).
- the WAP wash includes 1.5 min of agitation. This illustrates that we can substitute parts of the mechanical action with another process such as alternating pressure in the cleaning of soiled fabrics/textiles.
- Redeposition is furthermore improved in comparison with the fine wash.
- WAP wash was performed as described above.
- the WAP procedure was modified for the wash shown in column 2 and 3.
- column 2 the periods of alternating pressure in the WAP procedure was substituted with a constant low pressure of ⁇ 0.5 bar.
- column 3 the periods of alternating pressure in the WAP procedure was substituted with a constant pressure of 0.2-0.3 bar. All other steps were the same for washing and rinsing.
- a WAP wash is performed until step 8. Now adjust the pressure to ⁇ 0.5 bar and leave it like that until time 5 minutes. Now recycle the suds by withdrawing the suds from the chamber by closing the inlet pin and adjust the pressure to 3 bar. Place the two outlet tubes into a 2 L beaker and open the two outlet pins and when the pressure is almost 0 then close the two outlet pins. (Remember to cover the opening with a wet cloth so no aerosols will come out into the air).
- a WAP wash is performed until step 8. Now adjust the pressure to 0.2-0.3 bar (make sure you still have at least a third of the foam left) and leave it like that until time 5 minutes. Now recycle the suds by withdrawing the suds from the chamber by closing the inlet pin and adjust the pressure to 3 bar. Place the two outlet tubes into a 2 L beaker and open the two outlet pins and when the pressure is almost 0 then close the two outlet pins. (Remember to cover the opening with a wet cloth so no aerosols will come out into the air).
- the wash performance is illustrated in FIG. 2 showing that alternating pressure result in a better wash performance as compared to washing at a constant pressure in the absence of alternating pressure.
- Beaker wash, beaker rinse and WAP rinse were performed as described above.
- the wash performance is illustrated in FIG. 3 showing that WAP rinse adds extra wash performance to the system. This is most probably because LAS is more effectively removed by the WAP rinse as indicated by the redeposition test in the table. Accordingly, other components than LAS is expected to be efficiently removed by WAP rinse.
- ballast fabric Two portions of each 25 g ballast fabric were WAP washed for 5 min in a 80% LAS solution (3.8 mg/ml in water) by following steps 1 to 8 of the WAP wash described above.
- ballast fabrics were rinsed by either by WAP rinse or by beaker rinse and aliquots of 20 ml were withdrawn from the third and last rinse solution for testing of the presence of residual LAS. As indicated in the table below further rounds of beaker rinse (4-6) were carried out from which aliquots were also tested for the presence of residual LAS. Analysis of LAS was done at 270 nm in a Lamda 2 spectrophotometer from Perkin Elmer.
- the wash performance is illustrated in FIG. 4 showing that WAP rinse is superior to beaker rinse.
- the results show that the amount of residual LAS in the third and last WAP rinse is less than that of the corresponding rinse solution carried out in a glass beaker with mechanical agitation (stirring with a spatula by hand). Further rounds of beaker rinsing (column 4, 5 and 6) decrease the amount of residual LAS but not to the level of WAP rinse (column 2).
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Textile Engineering (AREA)
- Detergent Compositions (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Cleaning In General (AREA)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US13/120,238 US20110191965A1 (en) | 2008-11-17 | 2009-11-13 | Method of cleaning an object |
Applications Claiming Priority (7)
Application Number | Priority Date | Filing Date | Title |
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EP08169257 | 2008-11-17 | ||
EP08169257.6 | 2008-11-17 | ||
US11571908P | 2008-11-18 | 2008-11-18 | |
EP08169318 | 2008-11-18 | ||
EP08169318.6 | 2008-11-18 | ||
PCT/EP2009/065110 WO2010055121A1 (en) | 2008-11-17 | 2009-11-13 | Method of cleaning an object |
US13/120,238 US20110191965A1 (en) | 2008-11-17 | 2009-11-13 | Method of cleaning an object |
Publications (1)
Publication Number | Publication Date |
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US20110191965A1 true US20110191965A1 (en) | 2011-08-11 |
Family
ID=42169663
Family Applications (1)
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US13/120,238 Abandoned US20110191965A1 (en) | 2008-11-17 | 2009-11-13 | Method of cleaning an object |
Country Status (11)
Country | Link |
---|---|
US (1) | US20110191965A1 (pt) |
EP (1) | EP2358936B1 (pt) |
JP (1) | JP5587901B2 (pt) |
CN (1) | CN102216509B (pt) |
AR (1) | AR074195A1 (pt) |
AU (1) | AU2009315653B2 (pt) |
BR (1) | BRPI0921846A2 (pt) |
CA (1) | CA2739726A1 (pt) |
MX (1) | MX2011005114A (pt) |
RU (1) | RU2519554C2 (pt) |
WO (1) | WO2010055121A1 (pt) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2531889C1 (ru) * | 2013-10-09 | 2014-10-27 | Виктор Вацлавович Фельчук | Способ чистки меховых изделий |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102533468A (zh) * | 2011-12-31 | 2012-07-04 | 广州市浪奇实业股份有限公司 | 含漆酶的植物基中性洗衣粉 |
WO2014037509A1 (en) * | 2012-09-07 | 2014-03-13 | Novozymes A/S | Method of drying textile using alternating pressure |
CN106948127B (zh) * | 2017-05-16 | 2020-10-16 | 孙树功 | 一种压力洗衣机及压力洗涤方法 |
CN109722845B (zh) * | 2017-10-31 | 2020-12-29 | 上海小吉互联网科技有限公司 | 一种单独投放酶制剂的洗涤方法 |
CN109652218A (zh) * | 2019-02-03 | 2019-04-19 | 南京林业大学 | 一种具有降解功能的蛋白类泡沫发生剂及其制备方法 |
MA56133A (fr) * | 2019-08-08 | 2022-04-13 | Kemin Ind Inc | Procédés de traitement de textiles avec de la mousse et processus associés |
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US5866524A (en) * | 1994-03-30 | 1999-02-02 | Procter & Gamble Company | Foamed cleaning compositions and method of treating textile fabrics |
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SU798207A1 (ru) * | 1978-12-25 | 1981-01-23 | Белорусский Проектно-Технологическийинститут "Белбыттехпроект" | Устройство дл приготовлени РАбОчиХ PACTBOPOB дл СТиРАльНыХМАшиН |
JPS59232581A (ja) * | 1983-06-17 | 1984-12-27 | 工藤 隆 | 家庭用洗濯機 |
JPS623115Y2 (pt) * | 1985-12-02 | 1987-01-23 | ||
JPH0616582Y2 (ja) * | 1987-10-08 | 1994-05-02 | ダイキン工業株式会社 | 泡洗浄機 |
KR940009947B1 (ko) * | 1991-10-21 | 1994-10-19 | 삼성전자 주식회사 | 삶는 세탁기의 세탁방법 |
JPH0574483U (ja) * | 1992-03-16 | 1993-10-12 | 信雄 斯波 | 振動洗浄 |
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EP0679183B1 (en) * | 1992-12-01 | 2003-04-16 | Novozymes A/S | Enhancement of enzyme reactions |
JPH10113493A (ja) * | 1996-10-14 | 1998-05-06 | Koichi Nishiyama | 減圧式洗濯機あるいは減圧式洗濯乾燥機 |
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2009
- 2009-11-13 EP EP09753096.8A patent/EP2358936B1/en not_active Not-in-force
- 2009-11-13 AU AU2009315653A patent/AU2009315653B2/en not_active Ceased
- 2009-11-13 BR BRPI0921846A patent/BRPI0921846A2/pt not_active IP Right Cessation
- 2009-11-13 US US13/120,238 patent/US20110191965A1/en not_active Abandoned
- 2009-11-13 JP JP2011536024A patent/JP5587901B2/ja not_active Expired - Fee Related
- 2009-11-13 WO PCT/EP2009/065110 patent/WO2010055121A1/en active Application Filing
- 2009-11-13 MX MX2011005114A patent/MX2011005114A/es active IP Right Grant
- 2009-11-13 CN CN200980145639.6A patent/CN102216509B/zh not_active Expired - Fee Related
- 2009-11-13 CA CA2739726A patent/CA2739726A1/en not_active Abandoned
- 2009-11-13 RU RU2011124535/12A patent/RU2519554C2/ru not_active IP Right Cessation
- 2009-11-16 AR ARP090104433A patent/AR074195A1/es not_active Application Discontinuation
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US1838595A (en) * | 1930-11-05 | 1931-12-29 | Howard W Turner | Washing machine |
US2585464A (en) * | 1943-02-08 | 1952-02-12 | Hovden Havtor | Washing machine |
US4118189A (en) * | 1975-07-02 | 1978-10-03 | Henkel Kommanditgesellschaft Auf Aktien | Method of washing textiles |
US5866524A (en) * | 1994-03-30 | 1999-02-02 | Procter & Gamble Company | Foamed cleaning compositions and method of treating textile fabrics |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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RU2531889C1 (ru) * | 2013-10-09 | 2014-10-27 | Виктор Вацлавович Фельчук | Способ чистки меховых изделий |
WO2015053657A1 (ru) * | 2013-10-09 | 2015-04-16 | Виктор Вацлавович ФЕЛЬЧУК | Способ чистки меховых изделий |
Also Published As
Publication number | Publication date |
---|---|
RU2011124535A (ru) | 2013-01-27 |
CN102216509B (zh) | 2014-09-17 |
BRPI0921846A2 (pt) | 2016-01-12 |
CN102216509A (zh) | 2011-10-12 |
RU2519554C2 (ru) | 2014-06-10 |
CA2739726A1 (en) | 2011-04-05 |
EP2358936B1 (en) | 2014-03-12 |
WO2010055121A1 (en) | 2010-05-20 |
JP5587901B2 (ja) | 2014-09-10 |
AU2009315653A1 (en) | 2010-05-20 |
AR074195A1 (es) | 2010-12-29 |
AU2009315653B2 (en) | 2014-10-23 |
MX2011005114A (es) | 2011-06-16 |
JP2012508606A (ja) | 2012-04-12 |
EP2358936A1 (en) | 2011-08-24 |
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