EP2406423B1 - Fabric treatment composition and method - Google Patents
Fabric treatment composition and method Download PDFInfo
- Publication number
- EP2406423B1 EP2406423B1 EP10706576A EP10706576A EP2406423B1 EP 2406423 B1 EP2406423 B1 EP 2406423B1 EP 10706576 A EP10706576 A EP 10706576A EP 10706576 A EP10706576 A EP 10706576A EP 2406423 B1 EP2406423 B1 EP 2406423B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- fabric
- composition
- treatment composition
- fabric treatment
- clay
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Not-in-force
Links
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0036—Soil deposition preventing compositions; Antiredeposition agents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
- C11D3/1246—Silicates, e.g. diatomaceous earth
- C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2079—Monocarboxylic acids-salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/78—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon; with halides or oxyhalides of silicon; with fluorosilicates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/188—Monocarboxylic acids; Anhydrides, halides or salts thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/203—Unsaturated carboxylic acids; Anhydrides, halides or salts thereof
Definitions
- the present invention relates to a fabric treatment composition and a method of treatment of fabric.
- cleaning methods are directed towards effective cleaning of soils from the fabrics.
- Some cleaning formulations include soil release agents that make it easier for oily soils to be cleaned from fabrics.
- conventional cleaning formulations do not help much in reducing subsequent post-wash soiling of the fabric.
- One such method is a multi-step method of treating a fabric with a compound of alkaline earth metal, titanium or zinc, with a water-soluble compound of aluminium, and with C8-C24 soap, in presence of an aqueous carrier.
- the multi-step method disclosed therein is relatively less convenient and relatively less user-friendly.
- it must be communicated to the end-user to apply the ingredients to the fabric In a stepwise manner. End-users may not have adequate level of education to follow the instructions correctly and there is a need for a single step method for imparting hydrophobicity and reducing subsequent cleaning.
- EP-A1-0 244 500 discloses a water repellent composition being liquid at room temperature, which comprises a silicone oil and a substantially non-volatile paraffinic oil or low molecular weight hydrocarbon resin, wherein the separation index of the paraffinic oll or low molecular weight hydrocarbon resin to the silicone oil is at most 0.4.
- One of the objects of the present invention is to provide a method and a composition for treating a fabric to render the fabrics relatively more hydrophobic.
- Another object of the present invention is to provide a method and a composition for treating a fabric to impart relatively better stain-resistance to the fabric.
- composition comprising clay, silicone oil and fatty acid when contacted with a fabric in presence of water under specific pH conditions, renders the fabric hydrophobic.
- a fabric treatment composition comprising clay, silicone oil, and fatty acid, characterized in that
- a method of treatment of fabric comprising a step of contacting the fabric with the fabric treatment composition of the first aspect in presence of water.
- the fabric that can be treated includes synthetic as well as natural textiles. Fabrics may be made of cotton, polycotton, polyester, silk or nylon. It is envisaged that the method of the present invention can be used to treat garments and other clothing and apparel materials that form typical wash-load in household laundry.
- the household materials that can be treated according to the process of the present invention include, but are not limited to, bedspreads, blankets, carpets, curtains and upholstery.
- the process of the present invention is described primarily for treatment of a fabric, it is envisaged that the process of the present invention can be advantageously used to treat other materials such as jute, denim and canvass. It is envisaged that the process of the present invention can be used to treat articles such as shoes and jackets.
- the fabric treatment composition comprises at least 30% by weight of clay.
- the clay is preferably from 30% to 90%, more preferably from 50% to 90% by weight and most preferably from 60% to 85% by weight of the fabric treatment composition.
- the clay is a 2:1 clay.
- 1:1 clays that can be used include kaolinite, dickite, halloyside, nacrite, chrysolite, lizardite, and amesite.
- Preferred 2:1 clays are montmorrilonite, bentonite, and smectite.
- the silicone oil is preferably from 3% to 50%, more preferably from 3% to 30% by weight and most preferably from 5% to 10% by weight of the fabric treatment composition.
- Preferred silicone oil is polydimethylsiloxane.
- silicone oils examples include Q2-1607 (ex Dow Corning), 1107 (ex Dow Corning), SF8417 (ex Dow Corning), Q2-8166 (ex Dow Corning), 2-8630, Q2-8460 (ex Dow Corning), 3-0213 (ex Dow Corning), 2-8040 (ex Dow Corning) and ARA-222 (ex Dyetech, Inc), SM2125 (ex Momentive performance materials), SMW32 (ex Momentive performance materials), SM2059 (ex Momentive performance materials) and AN101 (ex Resil), AE104 (ex Resil) and AE112 (ex Resil).
- the fatty acid is preferably from 5% to 50%, more preferably from 5% to 30% by weight and most preferably from 5% to 20% by weight of the fabric treatment composition.
- the number of carbon atoms in the fatty acid is preferably from 8 to 50, more preferably from 10 to 48, most preferably from 12 to 22.
- the fatty acid is a saturated fatty acid.
- the saturated fatty acid is preferably selected from lauric acid, myristic acid, stearic acid, palmitic acid, or mixtures thereof.
- unsaturated fatty acids include oleic acid, linoleic acid, linoleinic acid, ricinoleic acid, elaidic acid, petroselenic acid, erucic acid, palmitoleic acid, myrostoleic acid, and 12-hydroxyoleic acid.
- Fatty acid may be directly added to the composition, Alternatively, it is envisaged that a corresponding fatty acid soap and an inorganic or organic acid are added to the composition for in situ generation of the fatty acid in the composition.
- the mass ratio of clay to fatty acid is greater than 1.
- pH of the fabric treatment composition refers to pH of a mixture obtained by adding 1 part of the fabric treatment composition to 99 parts of water. It is essential that pH of the composition is less than or equal to 6.
- the fabric treatment composition preferably comprises an acid other than the fatty acid in order to ensure that pH of the fabric treatment composition is less than or equal to 6.
- the acid other than fatty acid is preferably from 0.1 % to 20%, more preferably 0.5 to 10% and most preferably from 1% to 5% by weight of the fabric treatment composition.
- the composition may comprise a surfactant.
- the surfactant if present, is preferably not greater than 5%, more preferably not greater than 2% and most preferably not greater than 1% by weight of said composition.
- the fabric treatment composition may comprise other optional ingredients including fluorescer, perfume, and preservative.
- the method of treating fabric comprises a step of contacting the fabric with the fabric treatment composition in presence of water.
- the step of contacting the fabric with the fabric treatment composition in presence of water is at a pH less than or equal to 6.
- the pH may be maintained by adding an acid to the fabric treatment composition.
- an acid may be added during the step of contacting so as to ensure that the pH during the step of contacting the fabric is less than or equal to 6.
- Fabric treatment compositions were prepared by mixing clay, poydimethylsiloxane (Q2-1607 emulsion from Dow Corning) and fatty acid and adding citric acid solution to adjust pH to 5 unless specified otherwise.
- the % by weight of polydimethylsiloxane in the composition is given on water-free basis unless specified otherwise.
- the fabric treatment composition was added to water (1.4 g of the composition in 200 mL of water) to prepare an aqueous suspension.
- a fabric swatch (size 10 cm X 10 cm) made of desized cotton, polycotton or polyester (all obtained from Bombay Dyeing, India) was dipped in the above suspension. The liquor to cloth ratio of about three was maintained. After 15 minutes of soaking, the fabric swatch was removed from the suspension and dried at 40°C for about 1 hour. The dried swatches were then ironed.
- the fabric treatment composition comprising at least 30% clay provides hydrophobicity on cotton, polycotton and polyester swatches whilst the fabric treatment composition comprising less than 30% by weight provides hydrophobicity only on polyester swatches. It can be further seen that the hydrophobicity of treated fabrics improves as the mass ratio of clay to fatty acid in the composition exceeds 1.
- the fabric treatment compositions comprised stearic acid, silicone and sodium bentonite as tabulated below. All the treatments were at pH of 5. The results of evaluation of hydrophobicity are tabulated below. Table 5: Effect of amount of fatty acid in the composition Ex No Bentonite (% by weight) Stearic acid (% by weight) Silicone oil (% by weight) Hydrophobicity cotton polycotton polyester 12 86 9 5 Y Y Y 13 90 4.5 5.5 Y Y Y C 93 2 5 N Y Y
- the ompositions comprising at least 5% fatty acid by weight provide hydrophobicity on all substrates including cotton.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Detergent Compositions (AREA)
Description
- The present invention relates to a fabric treatment composition and a method of treatment of fabric.
- Any discussion of the prior art throughout the specification should in no way be considered as an admission that such prior art is widely known or forms part of the common general knowledge in the field.
- Conventional cleaning methods are directed towards effective cleaning of soils from the fabrics. Some cleaning formulations include soil release agents that make it easier for oily soils to be cleaned from fabrics. However, conventional cleaning formulations do not help much in reducing subsequent post-wash soiling of the fabric.
- On the other hand, various industrial treatments for fabric modification are known to render the fabric hydrophobic by lowering surface energy or by providing a surface texture with optimum roughness or by a combination of both the approaches. The fabric modification of this type is normally carried out during textile manufacture and involves elaborate processes using expensive chemicals such as fluoropolymers. Further, these processes are relatively difficult to be conveniently used in household.
- Thus there is an unfulfilled need for a fabric treating method that can be used in household for reduction of subsequent soiling of fabrics.
- One such method, disclosed in our pending application
1691/MUM/2007 -
EP-A1-0 244 500 discloses a water repellent composition being liquid at room temperature, which comprises a silicone oil and a substantially non-volatile paraffinic oil or low molecular weight hydrocarbon resin, wherein the separation index of the paraffinic oll or low molecular weight hydrocarbon resin to the silicone oil is at most 0.4. - It is an object of the present invention to overcome or ameliorate at least one of the disadvantages of the prior art, or to provide a useful alternative.
- One of the objects of the present invention is to provide a method and a composition for treating a fabric to render the fabrics relatively more hydrophobic.
- Another object of the present invention is to provide a method and a composition for treating a fabric to impart relatively better stain-resistance to the fabric.
- Present inventors have surprisingly found that a composition comprising clay, silicone oil and fatty acid when contacted with a fabric in presence of water under specific pH conditions, renders the fabric hydrophobic.
- According to a first aspect of the present invention there is provided a fabric treatment composition comprising clay, silicone oil, and fatty acid, characterized in that
- a. the composition comprises at least 30% by weight of clay, and
- b. pH of the composition is less than or equal to 6.
- According to a second aspect of the present invention there is provided a method of treatment of fabric comprising a step of contacting the fabric with the fabric treatment composition of the first aspect in presence of water.
- The fabric that can be treated includes synthetic as well as natural textiles. Fabrics may be made of cotton, polycotton, polyester, silk or nylon. It is envisaged that the method of the present invention can be used to treat garments and other clothing and apparel materials that form typical wash-load in household laundry. The household materials that can be treated according to the process of the present invention include, but are not limited to, bedspreads, blankets, carpets, curtains and upholstery. Although the process of the present invention is described primarily for treatment of a fabric, it is envisaged that the process of the present invention can be advantageously used to treat other materials such as jute, denim and canvass. It is envisaged that the process of the present invention can be used to treat articles such as shoes and jackets.
- The fabric treatment composition comprises at least 30% by weight of clay. The clay is preferably from 30% to 90%, more preferably from 50% to 90% by weight and most preferably from 60% to 85% by weight of the fabric treatment composition.
- Although any type of clay can be used, it is preferred that the clay is a 2:1 clay. 1:1 clays that can be used include kaolinite, dickite, halloyside, nacrite, chrysolite, lizardite, and amesite. Preferred 2:1 clays are montmorrilonite, bentonite, and smectite.
- The silicone oil is preferably from 3% to 50%, more preferably from 3% to 30% by weight and most preferably from 5% to 10% by weight of the fabric treatment composition. Preferred silicone oil is polydimethylsiloxane.
- Some examples of commercially available silicone oils that can be used include Q2-1607 (ex Dow Corning), 1107 (ex Dow Corning), SF8417 (ex Dow Corning), Q2-8166 (ex Dow Corning), 2-8630, Q2-8460 (ex Dow Corning), 3-0213 (ex Dow Corning), 2-8040 (ex Dow Corning) and ARA-222 (ex Dyetech, Inc), SM2125 (ex Momentive performance materials), SMW32 (ex Momentive performance materials), SM2059 (ex Momentive performance materials) and AN101 (ex Resil), AE104 (ex Resil) and AE112 (ex Resil).
- The fatty acid is preferably from 5% to 50%, more preferably from 5% to 30% by weight and most preferably from 5% to 20% by weight of the fabric treatment composition.
- The number of carbon atoms in the fatty acid is preferably from 8 to 50, more preferably from 10 to 48, most preferably from 12 to 22.
- Although both saturated and unsaturated fatty acids can be used, it is preferred that the fatty acid is a saturated fatty acid. The saturated fatty acid is preferably selected from lauric acid, myristic acid, stearic acid, palmitic acid, or mixtures thereof.
- Examples of unsaturated fatty acids include oleic acid, linoleic acid, linoleinic acid, ricinoleic acid, elaidic acid, petroselenic acid, erucic acid, palmitoleic acid, myrostoleic acid, and 12-hydroxyoleic acid.
- Fatty acid may be directly added to the composition, Alternatively, it is envisaged that a corresponding fatty acid soap and an inorganic or organic acid are added to the composition for in situ generation of the fatty acid in the composition.
- Preferably the mass ratio of clay to fatty acid is greater than 1.
- pH of the fabric treatment composition refers to pH of a mixture obtained by adding 1 part of the fabric treatment composition to 99 parts of water. It is essential that pH of the composition is less than or equal to 6. The fabric treatment composition preferably comprises an acid other than the fatty acid in order to ensure that pH of the fabric treatment composition is less than or equal to 6. The acid other than fatty acid is preferably from 0.1 % to 20%, more preferably 0.5 to 10% and most preferably from 1% to 5% by weight of the fabric treatment composition.
- The composition may comprise a surfactant. However the surfactant if present, is preferably not greater than 5%, more preferably not greater than 2% and most preferably not greater than 1% by weight of said composition.
- The fabric treatment composition may comprise other optional ingredients including fluorescer, perfume, and preservative.
- The method of treating fabric comprises a step of contacting the fabric with the fabric treatment composition in presence of water.
- It is essential the step of contacting the fabric with the fabric treatment composition in presence of water is at a pH less than or equal to 6. The pH may be maintained by adding an acid to the fabric treatment composition. Alternatively, an acid may be added during the step of contacting so as to ensure that the pH during the step of contacting the fabric is less than or equal to 6.
- The invention will now be demonstrated with examples. The examples are for the purpose of illustration only and do not limit the scope of the invention in any manner.
- Fabric treatment compositions were prepared by mixing clay, poydimethylsiloxane (Q2-1607 emulsion from Dow Corning) and fatty acid and adding citric acid solution to adjust pH to 5 unless specified otherwise. The % by weight of polydimethylsiloxane in the composition is given on water-free basis unless specified otherwise. The fabric treatment composition was added to water (1.4 g of the composition in 200 mL of water) to prepare an aqueous suspension. A fabric swatch (size 10 cm X 10 cm) made of desized cotton, polycotton or polyester (all obtained from Bombay Dyeing, India) was dipped in the above suspension. The liquor to cloth ratio of about three was maintained. After 15 minutes of soaking, the fabric swatch was removed from the suspension and dried at 40°C for about 1 hour. The dried swatches were then ironed.
- Contact angle was measured using Kruss Contact Angle Measurement Unit. Fabric swatch (either treated or untreated) was placed and a 20 µL drop of deionized water was placed on the fabric using a syringe. Contact angle was determined using digital photographs captured at interval of 2 seconds for a period of 2 minutes. Fabric was rated as hydrophobic if the contract angle of greater than 90° of the drop was maintained for a period of 2 minutes. Fabric was rated as not hydrophobic if the drop spreaded on the fabric before 2 minutes.
- The fabric treatment compositions are tabulated below. All the fabric treatments were at pH 5. The results of evaluation of hydrophobicity are also tabulated below.
Table 1: Effect of amount of clay Ex No Sodium bentonite (% by weight) Stearic acid (% by weight) Silicone oil (% by weight) Clay/F atty acid ratio Hydrophobicity cotton polycotton polyester 1 79 16 5 5 Y Y Y 2 70 23 7 3 Y Y Y 3 43.5 43.5 13 1 N Y Y A 28 56 16 0.5 N N Y - From the results, it is clear that the fabric treatment composition comprising at least 30% clay provides hydrophobicity on cotton, polycotton and polyester swatches whilst the fabric treatment composition comprising less than 30% by weight provides hydrophobicity only on polyester swatches. It can be further seen that the hydrophobicity of treated fabrics improves as the mass ratio of clay to fatty acid in the composition exceeds 1.
- Fabrics were treated with a composition similar to the composition of Ex No 1 except that myristic acid was used instead of stearic acid. The treatments were carried out at different values of pH as tabulated below. All the experiments were at clay to fatty acid mass ratio of 5. The results of evaluation of hydrophobicity are tabulated below.
Table 2: Effect of pH during the treatment Ex No pH Hydrophobicity on cotton Hydrophobicity on polycotton Hydrophobicity on polyester 4 3 Y Y Y 5 4 Y Y Y 6 5 Y Y Y 7 6 Y Y Y B 7 Y N N - From the results, it is clear that the fabric treatment at a pH of 6 or less than 6 provides hydrophobicity on cotton, polycotton and polyester swatches whilst the fabric treatment at pH greater than 6 provides hydrophobicity only on cotton swatches.
- The treatment composition used in Ex No 8 is same as that used in Ex No 1 in all respects except that 1:1 clay was used instead of 2:1 clay. The treatment was at pH of 5. The results of evaluation of hydrophobicity are tabulated below. The results of Ex No 1 are reproduced below for convenience.
Table 3: Effect of type of clay Ex No Clay Hydrophobicity on cotton Hydrophobicity on polycotton Hydrophobicity on polyester 1 Sodium bentonite (2:1 clay) Y Y Y 8 Kaolinite (1:1 clay) N Y Y - From the results, it is clear that the fabric treatment composition comprising 2:1 clay provides hydrophobicity on cotton, polycotton and polyester swatches whilst the fabric treatment composition comprising 1:1 clay provides hydrophobicity only on polycotton and polyester swatches.
- The treatment compositions were same as those used in Ex No 1 except for the type of fatty acid used, which are given in the table below. All the treatments were at pH of 5. The results of evaluation of hydrophobicity are tabulated below.
Table 4: Effect of type of fatty acid Ex No Fatty acid Hydrophobicity on cotton Hydrophobicity on polycotton Hydrophobicity on polyester 9 Lauric acid Y Y Y 10 Palmitic acid Y Y Y 11 Oleic acid N Y Y - From the results, it is clear that the fabric treatment composition comprising saturated fatty acid provides hydrophobicity on cotton, polycotton and polyester swatches whilst the fabric treatment composition comprising unsaturated fatty acid provides hydrophobicity only on polycotton and polyester swatches.
- The fabric treatment compositions comprised stearic acid, silicone and sodium bentonite as tabulated below. All the treatments were at pH of 5. The results of evaluation of hydrophobicity are tabulated below.
Table 5: Effect of amount of fatty acid in the composition Ex No Bentonite (% by weight) Stearic acid (% by weight) Silicone oil (% by weight) Hydrophobicity cotton polycotton polyester 12 86 9 5 Y Y Y 13 90 4.5 5.5 Y Y Y C 93 2 5 N Y Y - It can be seen that the ompositions comprising at least 5% fatty acid by weight provide hydrophobicity on all substrates including cotton.
- Three types of stains were used, prepared using following method.
- 1. Mud stain - 1g red soil obtained locally from Bangalore India (average particle size 180 micron,) was suspended in 200 mL deionized water.
- 2. Ketchup stain - 5 mL Kissan® (Hindustan Unilever Limited) tomato sauce was mixed in 200 mL deionized water
- 3. Tea stain - 3 Taj Mahal® (Hindustan Unilever Limited) tea-bags (6 g total) were dipped in 300 mL deionized water maintained at 80 °C for 20 minutes.
- 1 mL of above staining solution was poured drop by drop (from a height of 0.5 cm) using a micropipette over treated (according to Ex No 1) and untreated fabric swatch placed on a flat surface inclined at 40° from the horizontal. The behaviour of drops was observed to vary between two extremes. In some cases the drop of the staining solution rolled off from the fabric and in some cases the staining solution spread completely on the fabric instead of rolling off. The resulting staining of fabric was evaluated by a panel of 7 persons, who graded the staining on a scale of 0 to 5, with a score of 0 indicating no staining and a score of 5 indicating maximum staining. A low score indicates high stain repellency and vice versa. The results of evaluation of stain repellency are tabulated below.
Table 6: Stain repellency of treated fabrics Mud Tea Ketchup Fabric type Treated Untreated Treated Untreated Treated Untreated Cotton 0.2 4.4 1.1 3.9 1.3 3.9 Polycotton 1.0 4.4 0.9 3.8 0.1 3.6 Polyester 2.5 4.4 1.6 3.3 1.8 3.2 - From the results, it can be seen that the fabrics treated by the method and the composition of the present invention have relatively higher stain-resistance.
- It will be appreciated that the method and composition of fabric treatment according to the present invention render the fabrics relatively more hydrophobic and impart relatively better stain-resistance to the fabric.
Claims (10)
- A fabric treatment composition comprising clay, silicone oil, and fatty acid, characterized in that:i) the composition comprises at least 30% by weight of clay, andii) pH of the composition is less than or equal to 6, wherein by the pH of the fabric treatment composition is meant the pH of a mixture obtained by adding 1 part of the fabric treatment composition to 99 parts of water.
- A fabric treatment composition as claimed in claim 1 wherein said clay is a 2:1 clay.
- A fabric treatment composition as claimed in claim 1 or claim 2 wherein said fatty acid is a saturated fatty acid.
- A fabric treatment composition as claimed in any one of the preceding claims wherein said fatty acid is from 5% to 50% by weight of the composition.
- A fabric treatment composition as claimed in any one of the preceding claims wherein the mass ratio of clay to fatty acid is greater than 1.
- A fabric treatment composition as claimed in any one of the preceding claims wherein said clay is from 30% to 90% by weight of the composition.
- A fabric treatment composition as claimed in any one of the preceding claims wherein said silicone oil Is from 3% to 50% by weight of the composition.
- A fabric treatment composition as claimed in any one of the preceding claims wherein the composition comprises a surfactant in an amount not greater than 5% by weight of said composition.
- A fabric treatment composition as claimed in any one of the preceding claims comprising from 0.1% to 20% by weight an acid other than the fatty acid.
- A method of treating fabric characterized in that it comprises a step of conlacting the fabric with the fabric treatment composition as claimed in any one of the claims 1-9 in presence of water.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IN508MU2009 | 2009-03-09 | ||
PCT/EP2010/051963 WO2010102882A2 (en) | 2009-03-09 | 2010-02-17 | Fabric treatment composition and method |
Publications (2)
Publication Number | Publication Date |
---|---|
EP2406423A2 EP2406423A2 (en) | 2012-01-18 |
EP2406423B1 true EP2406423B1 (en) | 2012-11-21 |
Family
ID=42136241
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP10706576A Not-in-force EP2406423B1 (en) | 2009-03-09 | 2010-02-17 | Fabric treatment composition and method |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP2406423B1 (en) |
CN (1) | CN102348846B (en) |
ES (1) | ES2400222T3 (en) |
WO (1) | WO2010102882A2 (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2016197146A1 (en) | 2015-06-05 | 2016-12-08 | Cornell University | Modified cellulosic compositions having increased hydrophobicity and processes for their production |
US11352740B2 (en) | 2016-05-24 | 2022-06-07 | Inv Performance Surfaces, Llc | Compositions for the treatment of articles, and articles treated therefrom |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61115988A (en) * | 1984-11-12 | 1986-06-03 | Mitsubishi Chem Ind Ltd | Water-repellant composition |
GB2388610A (en) * | 2002-05-17 | 2003-11-19 | Procter & Gamble | Detergent composition containing silicone and fatty acid |
GB0505618D0 (en) * | 2005-03-18 | 2005-04-27 | Unilever Plc | Fabric care compositions |
CN101326321A (en) * | 2005-12-12 | 2008-12-17 | 美利肯公司 | Stain repellant and release fabric conditioner |
-
2010
- 2010-02-17 WO PCT/EP2010/051963 patent/WO2010102882A2/en active Application Filing
- 2010-02-17 ES ES10706576T patent/ES2400222T3/en active Active
- 2010-02-17 CN CN2010800115880A patent/CN102348846B/en not_active Expired - Fee Related
- 2010-02-17 EP EP10706576A patent/EP2406423B1/en not_active Not-in-force
Also Published As
Publication number | Publication date |
---|---|
WO2010102882A2 (en) | 2010-09-16 |
ES2400222T3 (en) | 2013-04-08 |
CN102348846B (en) | 2013-09-11 |
WO2010102882A3 (en) | 2011-01-27 |
CN102348846A (en) | 2012-02-08 |
EP2406423A2 (en) | 2012-01-18 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP2358854B1 (en) | Method and composition for the treatment of a substrate | |
JP7065767B2 (en) | Hydrophobic extender for non-fluorinated surface effect coatings | |
US3644204A (en) | Agent for the post-treatment of washed laundry | |
EP3310889B1 (en) | Laundry pretreatment composition | |
EP2406423B1 (en) | Fabric treatment composition and method | |
AU2019345048B2 (en) | Home care compositions | |
DE69628239T2 (en) | Washing composition and use of polymer for cleaning and dirt resistance of an article | |
EP2142698B1 (en) | Granular materials for textile treatment | |
DE60119729T2 (en) | TEXTILE WEAKMAKER COMPOSITIONS CONTAINING CATIONIC SOFTWARE AND FATTY ACID AMIDE | |
EP3224335B1 (en) | Method for treating fabric having oily stains | |
EP2473589A1 (en) | Composition and process for treatment of a fabric | |
EP2283107A1 (en) | Process for treatment of a fabric | |
EP0960181B1 (en) | Carpet cleaning compositions having increased levels of aminopolycarboxylic acids as anti-resoiling agents | |
DE60105763T3 (en) | COMPOSITION TO TEXTILE CARE | |
US4170557A (en) | Process and composition for imparting anti-soil redeposition and soil release properties to polyester textile materials | |
DE2217813C3 (en) | Mixture for surface treatment as well as detergent and cleaning agent mixture containing the same | |
JPS583066B2 (en) | Sentaku no Saiorimono Ni Techiyosarel Ichijijitekiyogoreridatsuseifuyojiyushi | |
JP2020165045A (en) | Softener and washing method of fiber | |
JP2005126828A (en) | Dark coloring agent composition | |
JPH11279939A (en) | Scouring of textile fiber |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
17P | Request for examination filed |
Effective date: 20110816 |
|
AK | Designated contracting states |
Kind code of ref document: A2 Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO SE SI SK SM TR |
|
DAX | Request for extension of the european patent (deleted) | ||
GRAP | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOSNIGR1 |
|
GRAS | Grant fee paid |
Free format text: ORIGINAL CODE: EPIDOSNIGR3 |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO SE SI SK SM TR |
|
REG | Reference to a national code |
Ref country code: GB Ref legal event code: FG4D |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP |
|
REG | Reference to a national code |
Ref country code: AT Ref legal event code: REF Ref document number: 585143 Country of ref document: AT Kind code of ref document: T Effective date: 20121215 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R096 Ref document number: 602010003749 Country of ref document: DE Effective date: 20130117 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FG2A Ref document number: 2400222 Country of ref document: ES Kind code of ref document: T3 Effective date: 20130408 |
|
REG | Reference to a national code |
Ref country code: NL Ref legal event code: VDEP Effective date: 20121121 |
|
REG | Reference to a national code |
Ref country code: AT Ref legal event code: MK05 Ref document number: 585143 Country of ref document: AT Kind code of ref document: T Effective date: 20121121 |
|
REG | Reference to a national code |
Ref country code: LT Ref legal event code: MG4D |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: NO Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20130221 Ref country code: FI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: SE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: LT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: ES Payment date: 20130226 Year of fee payment: 4 Ref country code: FR Payment date: 20130311 Year of fee payment: 4 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: PL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: PT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20130321 Ref country code: LV Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: BE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: GR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20130222 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: AT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: BG Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20130221 Ref country code: DK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: EE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: CZ Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: RO Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: NL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 |
|
PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MC Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20130228 |
|
26N | No opposition filed |
Effective date: 20130822 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: MM4A |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R097 Ref document number: 602010003749 Country of ref document: DE Effective date: 20130822 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: HR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20130731 Ref country code: IE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20130217 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DE Payment date: 20130227 Year of fee payment: 4 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R119 Ref document number: 602010003749 Country of ref document: DE |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
GBPC | Gb: european patent ceased through non-payment of renewal fee |
Effective date: 20140217 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: CH Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20140228 Ref country code: LI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20140228 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: ST Effective date: 20141031 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R119 Ref document number: 602010003749 Country of ref document: DE Effective date: 20140902 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: GB Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20140217 Ref country code: FR Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20140228 Ref country code: DE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20140902 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FD2A Effective date: 20150528 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SM Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: CY Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: ES Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20140218 Ref country code: MK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: HU Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT; INVALID AB INITIO Effective date: 20100217 Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20130217 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IS Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20121121 Ref country code: IT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20140217 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: TR Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20140217 |