EP2231906B1 - Microfibre - Google Patents

Microfibre Download PDF

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Publication number
EP2231906B1
EP2231906B1 EP08870019.0A EP08870019A EP2231906B1 EP 2231906 B1 EP2231906 B1 EP 2231906B1 EP 08870019 A EP08870019 A EP 08870019A EP 2231906 B1 EP2231906 B1 EP 2231906B1
Authority
EP
European Patent Office
Prior art keywords
fibers
fibres
fibre
cellulosic
dtex
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.)
Active
Application number
EP08870019.0A
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German (de)
English (en)
Other versions
EP2231906A2 (fr
Inventor
Johann Leitner
Gert Kroner
Egon DÜNSER
Karin KÄMPF
Harald Schobesberger
Roland MÖSLINGER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Lenzing AG
Original Assignee
Lenzing AG
Chemiefaser Lenzing AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Lenzing AG, Chemiefaser Lenzing AG filed Critical Lenzing AG
Publication of EP2231906A2 publication Critical patent/EP2231906A2/fr
Application granted granted Critical
Publication of EP2231906B1 publication Critical patent/EP2231906B1/fr
Active legal-status Critical Current
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Classifications

    • 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
    • D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
    • 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
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • 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
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/04—Blended or other yarns or threads containing components made from different materials
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/20—Cellulose-derived artificial fibres
    • 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
    • Y10T428/249921—Web or sheet containing structurally defined element or component
    • 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
    • Y10T428/2913—Rod, strand, filament or 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
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/30—Woven fabric [i.e., woven strand or strip material]
    • Y10T442/3065—Including strand which is of specific structural definition
    • Y10T442/313—Strand material formed of individual filaments having different chemical compositions

Definitions

  • the present invention relates to a high strength cellulosic regenerate fiber having a single fiber titer of between 0.6 and 0.9 dtex, and yarns and sheets containing such regenerated fibers.
  • microfibers generally refers to fibers having a denier of less than 1.0 dtex or, depending on the density of the material, a diameter of 9 to 10 ⁇ m (FIG. Lexikon der Textilveredlung ", HK Rouette, 1995, Volume 2, pp. 1250 ff; Laumann Verlag, Duelm s). It is also known that fabrics made of microfibers are fundamentally softer than those made of coarser fibers.
  • FR 2764910 claims a method in which the delay should be hydraulic instead of mechanical. Viscose fibers are obtained with a linear density of 0.3 dtex. Details about the strength of these fibers are not included.
  • the US 3785918 also discloses the preparation of a blend of viscose fibers and microfibers using a spinning device according to the ejector principle.
  • the obtained microfibers should be used for papermaking. They are very uneven and therefore not suitable for textile applications.
  • the US 4468428 discloses the production of viscose fibers with a diameter of 8 microns using a spinneret with nozzle hole diameters of 20 microns. Such nozzle hole diameters are not sufficient for large-scale production operation Operational safety operable because it is both very quickly deposits on the spin bath side of the nozzle hole, including the uniformity of the fiber diameter and the spinning security suffers or the entire nozzle channel is clogged by dirt particles and therefore the fiber titer varies even more.
  • the CN 1418990 discloses the production of ultrafine viscose fibers by a special adjustment of the withdrawal forces and matched nozzle hole diameter.
  • the fibers obtained in this way have a titer of 0.56 to 0.22 dtex. The achieved strength of these fibers can not be found in the document.
  • the JP 2005187959 proposes to use cellulose from California cedar for the production of viscose staple fibers. This is to obtain fibers over a wide titer range between 0.2 and 30 den, which would also include microfibers. However, the range between 1.5 and 10 ⁇ m, ie outside the microfiber range, is preferred. For fiber strength no information is given.
  • the JP 58089924 discloses nonwoven ultrafine fiber webs having a single fiber diameter of 0.05-2 ⁇ m.
  • the fibers may be made by the viscose, cuprammonium or acetate process. It seems important that they can be burned. In particular, for textile applications such fine fibers are no longer suitable.
  • the US 3539678 describes a modified viscose process obtained with fibers having a high wet modulus, so-called HWM fibers. These should be producible in a titer range of 0.7 to 5.0.
  • the examples contain only fibers with a denier of 1.0 denier (corresponding to 1.1 dtex) with a dry strength of max. 2.93 g / den (corresponding to 25.9 cN / tex).
  • the GB 310944 discloses the production of filament yarns with a single fiber titer of at most 1 den by the Cuoxam method. For example, fibers of 0.7 denier and a dry strength of 2.64 g / den (corresponding to 23.3 cN / tex) can be achieved.
  • the cuoxam process has significant environmental problems and is therefore no longer used worldwide with one or two exceptions.
  • the WO 98/58102 proposes a lyocell method for the production of cellulose microfibers. It should be emphasized at this point that a lyocell process does not lead to cellulose regenerated fibers in the context of this application, since in the lyocell process, the cellulose is only physically dissolved and reprecipitated, while in the production of cellulose regenerated first a cellulose derivative, such as cellulose xanthogenate or - as in the case of the Cuprammoniumvons - a cellulose-metal complex is generated, which is regenerated in the course of the process back to pure, undissolved cellulose.
  • a cellulose derivative such as cellulose xanthogenate or - as in the case of the Cuprammoniumbacters - a cellulose-metal complex is generated, which is regenerated in the course of the process back to pure, undissolved cellulose.
  • Fibers are made with a Einzelmaschinetiter from 0.3 to 1.0 dtex, preferably 0.8 to 1.0 dtex.
  • a Einzelmaschinetiter from 0.3 to 1.0 dtex, preferably 0.8 to 1.0 dtex.
  • WO 2005/106085 US 2005-056956 . US 2002-148050 .
  • WO 01/86043 and the references cited therein describe various approaches to the preparation of cellulosic microfibers by modifying the lyocell method by meltblowing or centrifugal spinning.
  • the fibers obtained herewith have uneven titer and fiber length distributions, so they are not suitable for high quality textile and fiber technical applications are suitable.
  • the methods require at least one compared to the usual lyocell process completely new spinning apparatus.
  • the productivity of the spinning process is significantly higher than the productivity of the ring and rotor spinning processes.
  • the productivity of this spinning process is about 2.5 times higher compared to rotor spinning.
  • the productivity of this process is even higher by about a factor of 15.
  • Spun processes based on the Murata vortex principle require about 75-80 fibers in the yarn cross-section. This means that this spinning system is able to spin much finer yarns than the rotor spinning process.
  • the strength of yarns produced on the basis of the MVS process is at a significantly higher level compared to rotor yarns.
  • the MVS spinning process requires fibers whose fiber strength makes it possible to produce yarns with yarn strengths which ensure high productivity during further processing into knitted or woven fabrics.
  • the cellulosic microfibers described above are not suitable for processing in high-performance spinning processes because of their relatively low absolute strength. High-fine yarns made of these fibers, which are needed to produce the increasingly demanded from the market lightweight textiles made of cellulosic fibers, could therefore not be produced with modern high-performance spinning process.
  • the object was to provide a cellulosic fiber available, the current requirements for an economically and environmentally responsible manufacturing process as well as increased wearing comfort and improved appearance of the garment made from it is sufficient.
  • this fiber should be producible on existing production facilities.
  • the solution to this problem is a high-strength cellulosic regenerated fiber, which has a single fiber titer T (dtex) between 0.6 and 0.9, preferably between 0.6 and 0.8, a strength (B c ) in the conditioned state of B c (cN ) ⁇ 1.3 ⁇ T + 2T and a wet modulus (B m ) at an elongation of 5% in the wet state of B m (cN) ⁇ 0.5 * ⁇ T.
  • the fiber according to the invention preferably has a fineness-related strength in the conditioned state of at least 34.5 cN / tex.
  • the fineness-related wet modulus of this fiber is preferably at least 5.6 cN / tex.
  • a strength of 50.0 cN / tex and a wet modulus of 10.0 cN / tex are preferred.
  • the fiber according to the invention can analogously to in AT 287905 be prepared described methods.
  • the spinning parameters such as spinning mass output per nozzle hole and take-off speed must be adjusted according to the desired single-fiber titer.
  • the strength and modulus of the fibers according to the invention are substantially higher than those given in the US Pat AT 287905 was to be expected.
  • the fiber according to the invention is present as staple fiber, ie it is cut to a uniform length in the course of the production process.
  • Usual cutting lengths for staple fibers for the textile sector are between about 25 and 90 mm. Only such a uniform length of all fibers allows easy processing on the today in the textile chain usual machines with high productivity.
  • the present invention also provides a yarn of the fibers according to the invention.
  • a yarn is characterized by a higher softness compared to yarns of coarser denier fibers.
  • the yarns according to the invention have a higher strength.
  • such an inventive yarn in addition to the fibers of the invention also fibers of other origin, such as synthetic microfibers of polyester, polyamide or polyacrylic, other cellulosic fibers (eg cotton, especially combed cotton, lyocell, cupro, linen , Ramie, Kapok ....), fine fibers of animal origin such as alpaca, angora, cashmere, mohair and various silks.
  • Preferred embodiments of the present invention are yarns prepared by means of air spinning processes with a fineness of more than 200 dtex, preferably less than 118 dtex, more preferably less than 100 dtex.
  • the yarn of the invention may consist of 100% of the regenerated cellulosic fibers or additionally contain at least one or a mixture of several other fine fiber types of the above types.
  • the fibers according to the invention are particularly suitable for producing high-quality, finer, softer textile surfaces with particularly pleasant wearing properties, blends with further fiber types, such as synthetic microfibers of polyester, polyamide or polyacrylic, other cellulosic fibers (eg cotton, especially combed cotton, lyocell, cupro, linen, ramie, kapok ....), fine fibers of animal origin such as alpaca, angora, cashmere, mohair, various silks, into consideration.
  • synthetic microfibers of polyester, polyamide or polyacrylic other cellulosic fibers (eg cotton, especially combed cotton, lyocell, cupro, linen, ramie, kapok ....), fine fibers of animal origin such as alpaca, angora, cashmere, mohair, various silks, into consideration.
  • core yarns can be produced whose inner "core” consists of a different type of fiber than the outer "shell". It is for example possible to produce a yarn with a core of continuous filament of polyamide, polyester or elastane and a sheath of the fiber according to the invention and thus to combine mechanical and comfort properties of the two types of fibers.
  • an object of the present invention is a textile fabric containing the fibers according to the invention.
  • the fabric as well as the yarn according to the invention may also contain other fibers.
  • the sheet is preferably a woven or knitted fabric, but may in principle also be a nonwoven. For high-quality nonwovens, the use of fibers of uniform length and diameter as well as high strength can be of crucial importance.
  • the fibers according to the invention are particularly suitable for producing high-quality, finer, softer textile surfaces with particularly pleasant wearing properties
  • fabrics are involved a basis weight of less than 150 g / m 2 , but in particular less than 115 g / m 2, a preferred embodiment of the present invention.
  • These may consist of 100% of the cellulosic regenerated fibers or additionally contain at least one other fine type of fiber.
  • woven shirt and blouse fabrics with a weight per unit area of less than 100 g / m 2 from yarns of high-performance spinning processes such as rotor or airjet spinning processes are possible.
  • synthetic microfibers of polyester, polyamide or polyacrylic, other cellulosic fibers eg cotton, especially combed cotton, lyocell, cupro, linen, ramie, kapok ....
  • fine fibers of animal origin such as alpaca, Angora, cashmere, mohair, various silks, preferred mixing partners for the production of finest yarns and light-weight textiles.
  • One according to AT 287905 cellulosic staple fiber produced in a commercial production plant with a titer of 0.8 dtex, measured in accordance with the BISFA regulations, in the conditioned state has a strength of 36.3 cN / tex and a modulus (5% elongation) of 5.9 cN / tex on. From 100% of this fiber, yarns with Nm 100 (Ne 60), Nm 135 (Ne 80) and Nm 180 (Ne 100) were produced using the AirJet technology on an MVS spinning machine. They consistently had a significantly higher softness than a yarn made from commercially available Lenzing Modal® fiber.
  • the fiber according to the invention from Example 1 was spun into fine yarns with Nm 180 (Ne 100) for comparison with the known ring spinning and Siro processes (Table 1). It could be clearly stated that the AirJet yarns have an approximately comparable strength (Breaking Tenacity) and elongation (Breaking Elongation) showed as the ring or Siro yarns, which are known for high quality, but significantly lower productivity.
  • One in a pilot plant also according to AT 287905 prepared staple cellulosic fiber with a titer of 0.65 dtex, measured in accordance with the BISFA regulations, in the conditioned state, a strength of 36.4 cN / tex and a modulus (5% elongation) of 6.3 cN / tex.
  • a yarn made from this fiber also had a significantly higher softness than a yarn made from commercially available Lenzing Modal® fiber.

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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)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Artificial Filaments (AREA)
  • Woven Fabrics (AREA)
  • Knitting Of Fabric (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Claims (12)

  1. Fibre cellulosique régénérée à haute résistance, avec un titre de fibre unitaire T compris entre 0,6 et 0,9 dtex, de préférence entre 0,6 et 0,8 dtex, caractérisée en ce qu'elle présente une résistance (Bc) de Bc(cN) ≥ 1,3√T+2T à l'état conditionné et un module humide (Bm) de Bm(cN) ≥ 0,5*√T pour un allongement de 5 %.
  2. Fibre régénérée selon la revendication 1, la fibre régénérée étant une fibre discontinue.
  3. Fil contenant des fibres cellulosiques régénérées selon la revendication 1.
  4. Fil selon la revendication 3 fabriqué par filature à jet d'air, d'une finesse inférieure à 200 dtex (50 Nm), de préférence inférieure à 100 dtex (85 Nm), ou encore mieux inférieure à 100 dtex (100 Nm).
  5. Fil selon la revendication 3 constitué à 100 % de fibres cellulosiques régénérées.
  6. Fil selon la revendication 3 qui contient en outre au moins un autre type de fibre fine.
  7. Fil selon la revendication 6, chaque autre type de fibre étant sélectionné dans le groupe comprenant des microfibres synthétiques comme le polyester, le polyamide ou l'acrylique, d'autres fibres cellulosiques (comme le coton, en particulier des cotons peignés, le lyocell, le cupro, le lin, la ramie, le kapok) et des fibres fines d'origine animale comme l'alpaga, l'angora, le cashmere, le mohair et diverses soies.
  8. Étoffe contenant des fibres cellulosiques régénérées selon la revendication 1.
  9. Étoffe selon la revendication 8 avec un poids surfacique inférieur à 150 g/m2, ou encore mieux inférieur à 115 g/m2.
  10. Étoffe selon la revendication 8 constituée à 100 % de fibres cellulosiques régénérées.
  11. Étoffe selon la revendication 8 qui contient en outre au moins un autre type de fibre fine.
  12. Étoffe selon la revendication 11, chaque autre type de fibre étant sélectionné dans le groupe comprenant des microfibres synthétiques comme le polyester, le polyamide ou l'acrylique, d'autres fibres cellulosiques (comme le coton, en particulier des cotons peignés, le lyocell, le cupro, le lin, la ramie, le kapok), ainsi que des fibres fines d'origine animale comme l'alpaga, l'angora, le cashmere, le mohair et diverses soies.
EP08870019.0A 2008-01-11 2008-12-05 Microfibre Active EP2231906B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AT472008 2008-01-11
ATA619/2008A AT506268B1 (de) 2008-01-11 2008-04-17 Mikrofaser
PCT/AT2008/000432 WO2009086571A2 (fr) 2008-01-11 2008-12-05 Microfibre

Publications (2)

Publication Number Publication Date
EP2231906A2 EP2231906A2 (fr) 2010-09-29
EP2231906B1 true EP2231906B1 (fr) 2018-08-22

Family

ID=40845950

Family Applications (1)

Application Number Title Priority Date Filing Date
EP08870019.0A Active EP2231906B1 (fr) 2008-01-11 2008-12-05 Microfibre

Country Status (12)

Country Link
US (2) US20100291823A1 (fr)
EP (1) EP2231906B1 (fr)
JP (1) JP5693234B2 (fr)
KR (2) KR101598091B1 (fr)
CN (2) CN104630919B (fr)
AT (1) AT506268B1 (fr)
BR (1) BRPI0822141A2 (fr)
ES (1) ES2697527T3 (fr)
PT (1) PT2231906T (fr)
TR (1) TR201816622T4 (fr)
TW (1) TWI498463B (fr)
WO (1) WO2009086571A2 (fr)

Families Citing this family (7)

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CN102767004A (zh) * 2011-06-20 2012-11-07 上海水星家用纺织品股份有限公司 量子能纤维混纺纱线、由其制备的面料及该面料的制备方法
DE202013011959U1 (de) 2012-08-22 2014-12-15 Deutsche Institute Für Textil- Und Faserforschung Denkendorf Direktgesponnene Cellulosefasern, deren Herstellung und Verwendung
DE102012016714A1 (de) * 2012-08-22 2014-02-27 Deutsche Institute Für Textil- Und Faserforschung Denkendorf Celluloseregeneratfasern, deren Herstellung und Verwendung
US11034817B2 (en) 2013-04-17 2021-06-15 Evrnu, Spc Methods and systems for processing mixed textile feedstock, isolating constituent molecules, and regenerating cellulosic and polyester fibers
TWI667378B (zh) 2014-01-03 2019-08-01 奧地利商蘭精股份有限公司 纖維素纖維
EP3467163A1 (fr) 2017-10-06 2019-04-10 Lenzing Aktiengesellschaft Étoffe de doublure de filaments lyocellulaires
CN109825911B (zh) * 2019-01-16 2021-10-12 绍兴市厚发纺织有限公司 一种保温混纺纱及其制备方法

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AT506268B1 (de) 2014-08-15
BRPI0822141A2 (pt) 2015-06-30
WO2009086571A3 (fr) 2009-09-11
US20100291823A1 (en) 2010-11-18
KR20100112612A (ko) 2010-10-19
KR20150116906A (ko) 2015-10-16
KR101598091B1 (ko) 2016-03-08
TR201816622T4 (tr) 2018-11-21
US20150159302A1 (en) 2015-06-11
JP5693234B2 (ja) 2015-04-01
AT506268A1 (de) 2009-07-15
WO2009086571A2 (fr) 2009-07-16
EP2231906A2 (fr) 2010-09-29
PT2231906T (pt) 2018-11-29
TW200951253A (en) 2009-12-16
TWI498463B (zh) 2015-09-01
ES2697527T3 (es) 2019-01-24
CN104630919A (zh) 2015-05-20
CN104630919B (zh) 2019-01-11
JP2011509356A (ja) 2011-03-24
US11932969B2 (en) 2024-03-19
CN101970732A (zh) 2011-02-09

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