WO2006060835A1 - Cellulosic staple fiber and its use as a filling material - Google Patents
Cellulosic staple fiber and its use as a filling material Download PDFInfo
- Publication number
- WO2006060835A1 WO2006060835A1 PCT/AT2005/000493 AT2005000493W WO2006060835A1 WO 2006060835 A1 WO2006060835 A1 WO 2006060835A1 AT 2005000493 W AT2005000493 W AT 2005000493W WO 2006060835 A1 WO2006060835 A1 WO 2006060835A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- fiber
- dtex
- cellulosic staple
- fibers
- staple fiber
- Prior art date
Links
Classifications
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/22—Yarns or threads characterised by constructional features, e.g. blending, filament/fibre
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B68—SADDLERY; UPHOLSTERY
- B68G—METHODS, EQUIPMENT, OR MACHINES FOR USE IN UPHOLSTERING; UPHOLSTERY NOT OTHERWISE PROVIDED FOR
- B68G1/00—Loose filling materials for upholstery
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/23907—Pile or nap type surface or component
- Y10T428/2395—Nap type surface
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2904—Staple length fiber
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2904—Staple length fiber
- Y10T428/2907—Staple length fiber with coating or impregnation
Definitions
- the present invention relates to the field of filling materials for textile objects such as duvets, cushions, pillows, mattresses, fleeces for upholstery, clothing and the like, and to materials which are especially useful therefor.
- filling materials for textile objects must meet special requirements. Especially, high bulk with a low density at the same time, and suitable properties with regard to heat insulation, moisture adsorption and moisture transport are desired.
- WO 99/16705 proposes a filling material consisting of a non-woven mixture of polyester fibers and Lyocell fibers.
- Lyocell fibers are cellulosic fibers which are spun from a solution of cellulose in an aqueous tertiary amine oxide, especially N-methyl-N-morpholine-N-oxide (NMMO).
- NMMO N-methyl-N-morpholine-N-oxide
- EP 1 067 227 Al discloses a mixed fiber fleece of polyester fibers and viscose fibers as a filling material.
- the known filling materials be it that they consist of one single fiber type or of fiber mixtures, or of mixtures of fibers with other materials, e.g. down, are still not fully satisfactory with regard to their properties.
- this object is achieved by the use of a multilobal cellulosic staple fiber, and, especially, by the use of the cellulosic staple fiber according to the present invention, as a filling material.
- a further aspect of the present invention relates to a filling material containing a multilobal cellulosic staple fiber, especially the cellulosic staple fiber according to the present invention.
- the present invention is based on the discovery that multilobal cellulosic staple fibers are excellently suitable as a filling fiber for various textile uses, especially for duvets, cushions, pillows, mattresses, fleeces for upholstery, clothing and the like.
- multilobal cellulosic staple fibers fibers are to be understood the cross-section of which exhibits three or more lobes.
- Such fibers can be produced by spinning a cellulose spinning solution through spinnerets, the openings of which exhibit three or more lobes having a ratio between length and width of the lobes of preferably 2:1 or more, respectively.
- the fibers thus produced exhibit a cross-section which, throughout the plurality of fibers, is substantially the same.
- multilobal cellulosic staple fibers possess a spectrum of properties which renders them particularly useful as a filling material.
- fibers of this kind exhibit a high flexural stiffness, high bulk, high rebound capacity and a high water absorption capacity.
- the titer of the multilobal cellulosic staple fiber used according to the present invention is 1.0 to 30 dtex, preferably more than 3.0 dtex, especially more than 5.0 dtex, preferably 5.6 to 10 dtex, especially preferred more than 6.0 dtex, especially 6.3 to 10 dtex.
- the suitable range of titers in each case depends on the envisaged use of the filling material.
- a lower decitex in the range of 1 dtex to 5 dtex, preferably about 3 dtex to 4 dtex is advantageous.
- a typical titer for textile applications is in the range of about 3.3 dtex.
- a titer in the range of from more than 5.0 dtex to 10 dtex is preferred.
- a typical titer lies in the range of about 6.7 dtex.
- a filling fiber is a cellulosic staple fiber, which is characterized in that
- the cross-section of the fiber has three or more lobes
- the titer of the fiber is 1.0 to 30 dtex, preferably more than 3.0 dtex, especially more than 5.0 dtex, preferably 5.6 to 10 dtex, especially preferred more than 6.0 dtex, especially 6.3 to 10 dtex
- This multilobal cellulosic staple fiber is a so-called "Modal” fiber.
- the term "Modal fiber” is a generic name by which according to the definition of BISFA (Bureau for the International Standardization of Man-Made-Fibers) a cellulosic fiber with a high wet tenacity and a high wet modulus (i.e. the force which is required to elongate the fiber in the wet condition by 5%) is to be understood.
- BISFA Bos for the International Standardization of Man-Made-Fibers
- a cellulosic fiber with a high wet tenacity and a high wet modulus i.e. the force which is required to elongate the fiber in the wet condition by 5%
- the multilobal cellulosic staple fiber according to the present invention possesses a spectrum of properties which excellently fulfils the requirements which are to be met by a filling fiber. Especially the higher flexural stiffness as compared with common Modal fibers is to be mentioned.
- a common Modal fiber with a titer of 6.5 dtex exhibits a flexural stiffness of 0.35 mN mnvVtex 2
- a multilobal Modal fiber according to the present invention exhibits, with the same titer, a flexural stiffness of 0.44 mN mnrVtex 2 .
- the flexural stiffness is measured by a method developed by the applicant.
- the measured value is displayed as the relation of the gradient of the force to path over a linear measuring range, based on the titer.
- a conditioned fiber is clamped into a clamping bar and cut with a cutting device to a length of exactly 5 mm.
- the clamping bar is moved upwardly at constant speed by an electric gear.
- the fiber is pressed onto a small sensor plate which is adapted to a force sensor.
- the stiffer the fiber the higher is the measured force. Due to the lack of possibilities to calibrate, no effective force is given for the calculation of the flexural stiffness.
- the numeric relation between area F of the fiber cross-section and the perimeter U of the fiber cross-section is preferably from 1.7:1 to 3.5:1.
- the lobes of the fiber cross-section are comparatively thicker and shorter.
- the numeric relation between the area of the cross-section of the fiber and the perimeter of the fiber can be determined by software-based calculation from a micro- photograph of the fiber cross-section.
- the area of the fiber cross-section is larger by a factor of 2.30-fold or more, preferably 2.50-fold or more, especially preferred 2.70-fold and more, than the area of the largest equilateral triangle which is inscribed into said cross-section. This resembles a more distinct development of the form of the lobes of the fiber.
- the ratio between the area of the fiber cross-section and the area of the largest equilateral triangle that can be inscribed, is determined by the method which is described in detail in WO 04/85720. This ratio is, in the following, referred to as the "Delta- factor".
- the multilobal Modal staple fibers according to the invention exhibit a very high water absorption capacity.
- the fiber according to the invention exhibits a Syngina absorption capacity of more than 6.0 g/g, preferably 6.5 g/g or more, especially preferred 6.8 g/g and more.
- the Syngina absorption capacity is calculated according to the test method disclosed in WO 04/85720.
- the fiber exhibits on its surface a substance increasing the slippage, especially silicone.
- a substance increasing the slippage especially silicone.
- Such substances can be applied in a manner known per se during the fiber production in the baths of the after-treatment and finishing steps.
- the multilobal Modal fiber according to the invention is not only suitable as a filling fiber but can also be used for other textile applications, such as e.g. for yarns and the like, in the common titer range of from 1.0 dtex to 5.0 dtex. Thereby, voluminous and bulky yarns can be produced, for example. These yarns are characterized by an increased air lock, an improved area coverage, a better moisture transport and an increased heat insulation.
- the cellulosic staple fiber according to the invention is outstandingly useful as a material for carpets or carpeted floors.
- the titer range of the fiber is preferably about 6.0 dtex or more.
- a process for the production of Modal fibers not having a lobal cross-section is known e.g. from AT 287.905 B. If, when carrying out such a process, a spinneret with multilobal, preferably trilobal openings is used, the multilobal Modal fibers according to the invention can be produced. Preferably, spinnerets with openings the lobes of which have a ratio of length to width of lower than 3:1 are used.
- the filling material which can be obtained by using a multilobal cellulosic staple fiber, especially the multilobal Modal fiber according to the invention, may be present in the form of a fleece, a fiberball, a wadding, or in other forms known to the skilled artisan.
- the filling material according to the invention essentially consists of the multilobal cellulosic staple fiber.
- the use of several components i.e. the multilobal cellulosic staple fiber on the one hand, and further materials, such as e.g. further fibers and/or further filling components on the other hand is suitable as a filling material.
- the fiber which can be used as the further component may preferably be selected from the group consisting of synthetic fibers, especially polyester fibers, polyacrylic fibers, polyamide fibers, polylactate fibers; natural fibers, especially cotton, kapok, bast fibers, sisal, silk; man- made cellulosic fibers, especially viscose fibers, Modal fibers, Lyocell fibers; and/or animal hair, especially sheep wool, horsehair, rabbit wool, camel hair and cashmere.
- synthetic fibers especially polyester fibers, polyacrylic fibers, polyamide fibers, polylactate fibers
- natural fibers especially cotton, kapok, bast fibers, sisal, silk
- man- made cellulosic fibers especially viscose fibers, Modal fibers, Lyocell fibers
- animal hair especially sheep wool, horsehair, rabbit wool, camel hair and cashmere.
- a material of the group consisting of down and feathers may be selected.
- Polyester fibers and/or down are especially preferred as the further components for the filling material according to the invention. If several components are used, the multilobal cellulosic staple fiber is preferably present in an amount of from 20 weight% to 90 weight%, based on the whole filling material.
- the components may be present mixed with another as a so-called "intimate mixture”.
- assemblies which are composed of various fleece-like layers.
- the multilobal cellulosic staple fiber (as a pure material or, again, mixed with another component) is used in at least one of these fleece-like layers.
- the multilobal cellulosic staple fiber may also be used in a modified form, e.g. inherently flame-retardant by incorporation of a flame- retardant agent (such as Exolit® 5060 by Messrs. Clariant), aftertreatment with a flame- retardant agent or otherwise modified in a flame-retardant fashion.
- a flame- retardant agent such as Exolit® 5060 by Messrs. Clariant
- the clay component may preferably comprise a montmorillonite or a modified or unmodified hectorite clay.
- the multilobal cellulosic staple fiber may, furthermore, be modified by a compound selected from the group consisting of chitosan and chitosonium polymers. Especially, it is advantageous to modify the fiber by coating the fiber with chitosan.
- chitosonium polymers to modify Lyocell fibers is known from WO 2004/007818.
- Multilobal cellulosic staple fibers modified with chitosan or a chitosonium polymer exhibit the known properties of chitosan, i.e. antimicrobial activity, positive influence on wound healing, odour repressive properties and antiallergenic properties, rendering these fibers especially useful as a filling material.
- figures 1 and 2 show fiber cross-sections of multilobal Modal fibers according to the invention, which have been produced according to example 1 and example 3, respectively.
- Figure 3 shows fiber cross-sections of multilobal Modal fibers which have been produced according to example 4.
- Viscose pulp with an R18-content of 93% was alkalized with mashing lye containing 240 g/1 sodium hydroxide under stirring at 35 0 C. Addition of the pulp and discharging of the slurry were performed continuously via a pump. The slurry was pressed off to a fleece of alkalized cellulose containing 33% cellulose and 17% sodium hydroxide.
- the fleece of alkalized cellulose was shredded.
- the alkalized cellulose was ripened at a temperature of 30°C, so that the copper viscosity of the cellulose was 16 mPa.s before sulfidizing.
- CS 2 based on cellulose
- sulfidation was performed in a sulfidation plant at 28°C for two hours while circulating the mass.
- the xanthogenate was dissolved with a dilute sodium hydroxide solution to a viscose with 6.1% cellulose, 6.5% NaOH and 36% CS 2 , based on cellulose.
- the viscose was filtered three times and de-aerated. 1 hour before spinning 3.0%, based on cellulose, of a modifying agent (ethoxylated amines) effecting a mantle structure were added to the viscose.
- the viscose was ripened to a spinning gamma value of 57. Viscosity during spinning was 80 ball-fall seconds.
- the viscose was spun on a commercial spinning device through spinnerets with 625 trilobal holes, each having 3 lobes of 72 x 33 ⁇ m (ratio of length to width: 2.18), into a spinning bath having the following composition:
- the spinning tow was cut to staples with a length of 60 mm, which then were fully regenerated in diluted sulfuric acid, thereafter washed with hot water until they were acid- free, desulfurized with dilute sodium lye, again washed, bleached with dilute sodium hypochlorite solution, again washed, finished with a silicone emulsion, pressed off and dried.
- Figure 1 shows fiber cross-sections of the fibers spun according to example 1.
- the fibers having a titer of 7.6 dtex, had the following properties:
- Fiber tenacity (wet state) 19 cN/tex Elongation (conditioned): 17%
- a hardwood pulp with an R18-content of 94% was alkalized with mashing lye containing 220 g/1 sodium hydroxide under stirring at 45 0 C. Further treatment of the slurry and sulfidation were performed in the same manner as described in example 1. The xanthogenate was dissolved with a dilute sodium hydroxide solution to a viscose with 5.9% cellulose, 6.1% NaOH and 36% CS 2 , based on cellulose.
- the fibers having a titer of 6.1 dtex, had the following properties:
- Fiber tenacity (wet state) 19 cN/tex
- An eucalyptus pulp with an R18-content of 97.5% was alkalized with mashing lye containing 220 g/1 sodium hydroxide under stirring at 50 0 C. Further treatment of the slurry and sulfidation were performed in the same manner as described in example 1. The xanthogenate was dissolved with a dilute sodium hydroxide solution to a viscose with 6.1% cellulose, 6.2% NaOH and 36% CS 2 , based on cellulose.
- the fibers having a titer of 3.3 dtex, had the following properties:
- Fiber tenacity (wet state) 18 cN/tex
- Figure 3 shows fiber cross-sections of the fibers spun according to example 4.
- Example 5
- fleeces were produced which were used as a filling material for duvets.
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Nonwoven Fabrics (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Bedding Items (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
Abstract
Description
Claims
Priority Applications (14)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007544683A JP5348892B2 (en) | 2004-12-10 | 2005-12-07 | Cellulose staple fiber and its use as filler |
NZ555694A NZ555694A (en) | 2004-12-10 | 2005-12-07 | Cellulosic staple fiber and its use as a filling material |
AU2005313828A AU2005313828B2 (en) | 2004-12-10 | 2005-12-07 | Cellulosic staple fiber and its use as a filling material |
BRPI0519003A BRPI0519003B1 (en) | 2004-12-10 | 2005-12-07 | use of a plurality of multilobulated cellulosic fibers and filler |
ES05814935.2T ES2551100T3 (en) | 2004-12-10 | 2005-12-07 | Filling material and use of cellulosic cut fibers as filler fiber |
EP05814935.2A EP1819851B1 (en) | 2004-12-10 | 2005-12-07 | Filling material and use of cellulosic staple fibers as filling fibre |
CN2005800423700A CN101076620B (en) | 2004-12-10 | 2005-12-07 | Short fiber of cellulose and its application as filling material |
PL05814935T PL1819851T3 (en) | 2004-12-10 | 2005-12-07 | Filling material and use of cellulosic staple fibers as filling fibre |
CA 2589461 CA2589461C (en) | 2004-12-10 | 2005-12-07 | Cellulosic staple fiber and its use as a filling material |
US11/810,522 US20080090076A1 (en) | 2004-12-10 | 2007-06-06 | Cellulosic staple fiber and its use |
KR1020077012799A KR101343016B1 (en) | 2004-12-10 | 2007-06-07 | Cellulosic staple fiber and its use as a filling material |
US12/649,851 US20100104867A1 (en) | 2004-12-10 | 2009-12-30 | Cellulosic Staple Fiber and Its Use |
US13/095,438 US20110200783A1 (en) | 2004-12-10 | 2011-04-27 | Cellulosic staple fiber and its use |
US13/724,306 US20130189474A1 (en) | 2004-12-10 | 2012-12-21 | Cellulosic staple fiber and its use |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AT20832004 | 2004-12-10 | ||
ATA2083/2004 | 2004-12-10 | ||
ATA256/2005 | 2005-02-17 | ||
AT0025605A AT501931B1 (en) | 2004-12-10 | 2005-02-17 | CELLULOSE STAPLE FIBER AND ITS USE |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US11/810,522 Continuation US20080090076A1 (en) | 2004-12-10 | 2007-06-06 | Cellulosic staple fiber and its use |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2006060835A1 true WO2006060835A1 (en) | 2006-06-15 |
Family
ID=36013253
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/AT2005/000493 WO2006060835A1 (en) | 2004-12-10 | 2005-12-07 | Cellulosic staple fiber and its use as a filling material |
Country Status (15)
Country | Link |
---|---|
US (4) | US20080090076A1 (en) |
EP (1) | EP1819851B1 (en) |
JP (2) | JP5348892B2 (en) |
KR (1) | KR101343016B1 (en) |
CN (1) | CN101076620B (en) |
AT (1) | AT501931B1 (en) |
AU (1) | AU2005313828B2 (en) |
BR (1) | BRPI0519003B1 (en) |
CA (1) | CA2589461C (en) |
ES (1) | ES2551100T3 (en) |
NZ (1) | NZ555694A (en) |
PL (1) | PL1819851T3 (en) |
RU (1) | RU2388855C2 (en) |
TW (1) | TWI425125B (en) |
WO (1) | WO2006060835A1 (en) |
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WO2008019412A2 (en) * | 2006-08-14 | 2008-02-21 | Lenzing Aktiengesellschaft | Use of a cellulosic fibre in fillings |
US20100021711A1 (en) * | 2006-06-14 | 2010-01-28 | Lenzing Aktiengesellschaft | Lyocell Staple Fiber |
WO2011026160A1 (en) | 2009-09-03 | 2011-03-10 | Lenzing Ag | Cellulose fibres having an improved dosing ability, method for the production thereof and use thereof for reinforcing composite materials |
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Also Published As
Publication number | Publication date |
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AT501931A1 (en) | 2006-12-15 |
BRPI0519003B1 (en) | 2015-11-24 |
US20130189474A1 (en) | 2013-07-25 |
ES2551100T3 (en) | 2015-11-16 |
US20110200783A1 (en) | 2011-08-18 |
US20100104867A1 (en) | 2010-04-29 |
KR20070085835A (en) | 2007-08-27 |
TW200634187A (en) | 2006-10-01 |
CA2589461C (en) | 2013-02-12 |
AU2005313828A1 (en) | 2006-06-15 |
US20080090076A1 (en) | 2008-04-17 |
RU2007120348A (en) | 2009-01-20 |
PL1819851T3 (en) | 2015-12-31 |
CN101076620B (en) | 2013-05-01 |
TWI425125B (en) | 2014-02-01 |
NZ555694A (en) | 2010-01-29 |
JP2013256748A (en) | 2013-12-26 |
EP1819851A1 (en) | 2007-08-22 |
AT501931B1 (en) | 2007-08-15 |
JP2008523258A (en) | 2008-07-03 |
BRPI0519003A2 (en) | 2008-12-23 |
AU2005313828B2 (en) | 2011-01-27 |
EP1819851B1 (en) | 2015-07-29 |
KR101343016B1 (en) | 2013-12-19 |
RU2388855C2 (en) | 2010-05-10 |
CN101076620A (en) | 2007-11-21 |
JP5348892B2 (en) | 2013-11-20 |
CA2589461A1 (en) | 2006-06-15 |
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