EP1791996A1 - Procede de preparation d'une structure cellulosique non- tissee et structure cellulosique non-tissee ainsi preparee - Google Patents

Procede de preparation d'une structure cellulosique non- tissee et structure cellulosique non-tissee ainsi preparee

Info

Publication number
EP1791996A1
EP1791996A1 EP05823538A EP05823538A EP1791996A1 EP 1791996 A1 EP1791996 A1 EP 1791996A1 EP 05823538 A EP05823538 A EP 05823538A EP 05823538 A EP05823538 A EP 05823538A EP 1791996 A1 EP1791996 A1 EP 1791996A1
Authority
EP
European Patent Office
Prior art keywords
woven
filaments
cellulosic structure
aforesaid
woven cellulosic
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.)
Withdrawn
Application number
EP05823538A
Other languages
German (de)
English (en)
Inventor
Jagrat Maheshprasad Aditya Birla Centre MANKAD
Parag Dilip Aditya Birla Centre PATIL
Aditya Narayan Shrivastava
Brij Bhusan Koutu
Raj Kumar Ojha
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.)
Birla Research Institute for Applied Sciences
Original Assignee
Birla Research Institute for Applied Sciences
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 Birla Research Institute for Applied Sciences filed Critical Birla Research Institute for Applied Sciences
Publication of EP1791996A1 publication Critical patent/EP1791996A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/015—Natural yarns or filaments
    • 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
    • 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
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/013—Regenerated cellulose series
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments

Definitions

  • the present invention relates to a process for preparing a non-woven cellulosic structure and the non-woven cellulosic structure prepared therefrom. Particularly, the present invention relates to a process for preparing a consolidated multiple / single layer, absorbent, durable or disposable composite non-woven cellulosic structure comprising of at least one layer that is made from bio ⁇ degradable, continuous cellulosic material.
  • the present invention relates to a process for preparing a non-woven cellulosic structure comprising of continuous, randomized cellulosic fibers and the composite non-woven cellulosic structure prepared therefrom.
  • Consolidated non-woven structure may comprise of Viscose Fibers, Lyocell Fibers, Cellulose acetate, and / or its blends with synthetic fibers.
  • Lyocell fiber is a man made fiber based on dissolving non-derivatized cellulose directly in an organic solvent. Lyocell fibers are produced by regeneration of cellulosic fiber from a solution of cellulose in an organic solvent like N Methyl Morpholine N Oxide.
  • U.S. Patent 3600379 discloses a process of manufacturing Viscose fibers wherein the wood pulp is utilized as a raw material. It is steeped either as sheets or slurry with 17 - 22 percent NaOH solution. The excess steeping liquor is removed by pressing. The alkali cellulose is shredded and aged. The aged alkali cellulose is xanthated with an amount of carbon disulphide. The xanthate is dissolved in NaOH solution forming Viscose solution. The viscose is ripened and filtered once or several times either during or after ripening.
  • the viscose solution can then be spun through fine orifices in acidic spin bath to form regenerated cellulosic filaments / fibers / tow.
  • Viscose / Rayon spinning is almost 100 years old technology and hence described in brief only. Similarly preparation of non-derivatized cellulose solution through solvent spinning route is also known.
  • Indian Patent No. 189773 mentions a " process of preparing cellulose solution for spinning fibers / films.
  • the process includes introducing cellulose material into an aqueous solution of tertiary amine oxide to prepare a suspension. Later the suspension is subjected to high shear equipment heating under reduced pressure.
  • US Patent 4,144,080 and 4,246,221 disclose a method of preparation of amine oxide solution by extruding ground tertiary Amine Oxide solution and Cellulose. Also disclosed is the method of producing fibers by spinning the solution through fine orifices in air, orienting the same by mechanical stretching and regenerating the cellulose from the solution by allowing the spun filaments to pass through a bath of a nonsolvent.
  • the tow is washed and fibers cut into staple length. Conventionally the staple fibres are dried and baled (if non-wovens are prepared at different location).
  • the dried staple fiber bale is opened, blended if required and carded to form a fibrous mat.
  • This mat is directly or after cross lapping bonded to form a non-woven material.
  • US Patents 3,620,903 and 4,069,563 disclose a method to produce light weight, non patterned non- woven fabrics by treating fibrous sheet of materials with fine, essentially one or more columnar streams of liquid jetted from orifices, under high pressure. A layer of fiber web is supported on a surface and traversed with the streams to entangle the fibers in a manner which imparts strength and stability without the need for binder.
  • the aforesaid patents describe the processes wherein the cellulosic solution is spun using a solvent spun method.
  • the cellulosic fibers are spun and cut into staple lengths. Subsequently, they are treated with water and/or other chemicals. These wet fibers are then dried.
  • the mat is opened by use of an opener, carded and then hydro entangled to obtain a spun laced product.
  • the said product is re-dried to achieve a cellulosic non-woven fiber.
  • This is a conventional and well-accepted method to produce cellulosic non- woven fiber.
  • the process involves drying the said fiber twice, thereby increasing the costs. Also strength of the said non- woven fiber is not high since it comprises of short (staple) length fibers. Summary of present invention
  • the present invention discloses a process of manufacturing continuous cellulosic filaments obviating the aforesaid drawbacks.
  • the present invention relates to a process for preparing a non-woven cellulosic structure comprising the steps of extruding filaments from a cellulosic solution; passing the extruded filaments through a regenerating liquid to attenuate the filaments and laying the attenuated filaments into a web and to the non-woven cellulosic structure prepared therefrom.
  • Figure 1 shows the isometric view of the assembly for spinning the non-woven cellulosic material.
  • Figure 2 shows the exploded isometric view of the spinning box as shown in Figure 2.
  • Figure 3 shows the isometric view of the set up showing the laying of the curtain.
  • Figure 4(a) to 4(e) show various options for preparation of a composite structure.
  • the cellulose solution at required temperature and constant flow rate is fed into a spinneret assembly (7), preferably a rectangular assembly.
  • a spinning box (3) is kept below the rectangular spinneret assembly.
  • the spinning box (3) is used to attenuate the filaments and also to randomly lay down the filaments, thereby maintaining the rectangular configuration of the web.
  • the regeneration liquid is fed with the help of a regeneration liquid feed pipe (4).
  • the location of the regeneration liquid feed pipe can be either from the top or from the bottom of the spinning box.
  • the spinning box (3) comprises of a funnel shaped sides which form a funnel shape till a certain length, the rest of the portion remaining straight.
  • the funnel is meant to allow the regeneration liquid to pass from top to bottom.
  • Top part of the funnel (5) may have perforations in the side plate so that as the regeneration liquid starts filling up the spinning box (3), the fluid comes out from the perforations and passes through the funnel.
  • Flow from the regeneration liquid feed pipe (4) is regulated to maintain a constant level of the liquid.
  • the height of the water column in the spinning box makes the liquid flow from the funnel (5) at a high speed, due to gravitational acceleration. High speed fluid imparts a drag to the filaments fed from the spinneret assembly and get attenuated. Stretched filaments are allowed to fall by way of its own energy gained by the fluid flow on to a collection belt conveyor (8).
  • the collection belt (8) moves at a slower speed as compared to the filament drop down speed, the filaments lay down randomly on the belt forming a fairly entangled non-woven web.
  • the entire conveyor is placed within a regeneration liquid collection tank (9).
  • the regeneration liquid by gravity flows out of this tank to the recovery section and the recycle section.
  • Laying is attained by a vacuum system (10), whihc is provided below the collection belt just under the filament outlet. Vacuum allows the filaments to retain its random orientation on the belt, thereby reducing the effect of water force.
  • FIG. 3 shows one of the preferred laying options.
  • Curtain (11) formed by the aforedescribed method is brought to the feeding box (12).
  • the feeding box may have a mechanically driven twin roll arrangement to draw the curtain and feed it below.
  • the feeding box (12) is pivoted by a swing arrangement, which lays down the curtain in folds (13) on to the moving collecting belt (14).
  • the speed of the swing the drop down rate and the belt conveyor speed can be adjusted.
  • one or more feeding boxes (12) in combination with collecting belt (14) may operate such that web structure like that of a cross lapper is obtained.
  • a cross lapped web may have a higher coverage and better tensile strength in cross direction (CD) as compared to the CD tensile strength of the web made as shown in Figure 3.
  • CD cross direction
  • Figure 4(a) shows a typical un-consolidated laid mat made from Viscose continuous filaments (1) randomized by fluid assisted randomizer.
  • Figure 4(b) shows a typical un-consolidated laid mat made from Lyocell continuous filaments (2) randomized by fluid assisted randomizer.
  • the above two structures may be consolidated by known methods described.
  • Figure 4(c) is a representative sketch of a non-woven composite structure prepared by the aforesaid process prior to consolidation.
  • the bottom layer is cellulosic non- woven Viscose or Lyocell or the like (1) or (2) prepared by the process described above, while the top layer may be either cellulosic non-woven or synthetic non-woven web (x).
  • the structure may be consolidated by known methods described above to form a consolidated structure.
  • Figure 4(d) is a representative sketch of a non- woven composite structure prepared by the process described above prior to consolidation.
  • the bottom layer may be either cellulosic non- woven or synthetic non- woven web (x), while the top layer is cellulosic non-woven Viscose or Lyocell or the like (1) or (2) prepared by the process described above.
  • the structure may be consolidated by known methods.
  • Figure 4(e) represents a composite structure with multiple layers of either cellulosic or synthetic non-wovens (xl , x2...) with at least one layer of cellulosic non- woven Viscose or Lyocell or the like (1) or (2) prepared by the process described above. Presence or absence of either of the layers (1) or (2) may be decided upon the desired performance of the composite structure.
  • the structure may then be consolidated by known methods.
  • Pulp preferred for use for making the solution is soft wood pulp having high alpha cellulose content (89-93%) and low hemi-cellulose content.
  • DP Degree of Polymerization
  • Cellulose concentration to achieve a spin able solution can be in the range of 5% to 28%.
  • Preferably 7% to 20%, most preferred values of the cellulose concentration are 10% to 15%.
  • NMMO N-Methyl Morpholine N-Oxide as available in the market is of 50% concentration has to be pre-concentrated to 77% prior to dissolution of cellulose by conventional distillation process.
  • Blending of small pieces of pulp with pre-concentrated solvent is carried out at about 100°C in a double blade sigma mixer where in vacuum of 400 mm Hg is applied. After duration of 1.5 hours a homogeneous solution is obtained, which is allowed to cool down to solid condition.
  • Other methods available for making cellulose solutions on a continuous basis are available like use of high shear blender, thin film device or a devolatalizing type counter rotating twin screw extruders. A method described in Indian Patent No. 189773 may also be followed.
  • the above given aspect ratio allows for providing 10 to 60 rows of holes.
  • Lyocell polymer During spinning of Lyocell polymer at 90 to 110 deg C, adequate air gap and air flow in cross direction is provided. Depending upon the size of the spinneret and the stretch ratio, filaments from sub denier to 5 deniers can be spun.
  • Filaments coming out in the form of a curtain retain their rectangular configuration by the virtue of a special device, which contains the regeneration bath.
  • Central portion of the box has a funnel type arrangement.
  • the funnel may be perforated from the top and plain below a certain distance. Internals are so arranged such that a slit is provided at the bottom of the funnel, which serves as an outlet for the regeneration solution as well as outlet for spun filament.
  • the funnel is sealed and isolated from the sides so that the regeneration liquid from the bottom of the box cannot enter the funnel.
  • the inlet of the regeneration liquid is provided at the bottom. As the liquid fills the box and level is raised beyond the plain portion of the funnel, the liquid reaches to the perforated portion of the funnel. Liquid enters the funnel. Flow in the box is so adjusted that the outlet level matches with the inlet and always keeps the regeneration box full up to the brim.
  • the velocity of the extruded filaments is 8m/min to 80m/min.
  • V 2 2 x g x h
  • V - velocity of regeneration liquid in m/sec V - velocity of regeneration liquid in m/sec.
  • the velocity of the regenerating liquid is kept between 50m/min to 250m/min, preferably between 1 OOm/min to 200m/min.
  • the filaments are attenuated.
  • the said filaments formed by the method described above are brought to the belt conveyor where filaments may get additionally randomized due to flow of regenerating liquid.
  • collection of web may be done on a rotary vacuum drum system.
  • the feeding box may have a mechanically driven twin roll arrangement to draw the web and feed it below.
  • the feeding box has a variable speed drive and is pivoted by a swing arrangement which lays down the web in folds on to the moving collecting belt. Step less adjustment of the swing amplitude and the swing speed can also be provided.
  • the amplitude of the swing the drop down rate and belt conveyor speed can be adjusted so as to get webs with coverage from 10 to 600 gsm. Filament mat can also be formed without swinging the feeding box also. Then the only variables would be the conveyor and the curtain drop down speed.
  • Yet another laying option is cross lapping.
  • the method is similar to the one shown in Figure 3. However, there are one or more 1 than one boxes feeding the belt conveyor in cross direction. Swing boxes lay down the web along the width of the conveyor giving a cross lapping type laying, as well as they may lay it along the direction of the moving belt conveyor as shown in Figure 3 if required, such a web may have higher coverage and better tensile strength in cross direction as compared to the CD tensile strength shown in Figure 3.
  • the laying options cited above are especially beneficial when cellulosic fibers are to be mixed with other fibers. When a composite structure is required, web of 1 or more fiber is brought in to form a multi layer structure. The resultant web would be a composite structure of cellulosic and the other fibers.
  • the un-bonded web then passes through consolidation step, which may include hydro-entanglement, chemical bonding, needle punching system, etc., which consolidates the mat fibers together to produce a bonded consolidated non- woven material.
  • consolidation step which may include hydro-entanglement, chemical bonding, needle punching system, etc., which consolidates the mat fibers together to produce a bonded consolidated non- woven material.
  • wet non-woven bonded material is thereafter treated for, bleaching, further washing, dyeing, soft finishing, etc. and then passed through a dryer that expels excess moisture. Subsequently the web is collected on the winder and rolled.
  • the said web has a soft handle and good strength and may be used for many different applications of semi-durable or disposable segment.
  • Lyocell route an air gap is maintained between the regeneration liquid and spinneret, while in case of Viscose route, spinneret is immersed in the regeneration bath, since Viscose spinning is a wet spinning process. Thus a viscose web is formed.
  • Cross section of the cellulosic fibers may be altered by using different spinnerets to obtain tri-lobal, Y-shaped, or other shapes to impart specific properties to the structure. Subsequent steps are same as mentioned above for the solvent spinning route for the formation of a non- woven material. Only the hydro entanglement / consolidation operating parameters might differ for Viscose.
  • the un-bonded non-woven structure is consolidated using various processes known to those skilled in the art. Process may include hydro entanglement, needle punching, thermal bonding, spot bonding, melt stabilization, latex or chemical bonding. Type of,bonding / consolidation process used may be decided based on the desired end product / product characteristics.
  • Test procedures used to determine the properties of the consolidated non- woven structure and products made by the disclosed process are known to those well versed in the non- woven field.
  • a sample of 200 mm length and 2.5cm wide can be stretched in an Instron equipment at a rate of 100 mm/min obtains the point at which the structure yields.
  • This figure when represented in N/2.5cm value describes the value of tensile strength of a non-woven. Values obtained are shown in the table A/o- I ,.
  • This test is a measure of randomization of filaments in a non-woven structure.
  • Example 1 12% cellulose Lyocell polymer solution was fed at the rate of 0.06 grams/hole/min through a rectangular spinneret having 20 rows of 80 micron diameter holes, giving an extrusion speed of 10 m/min. Below the spinneret the spinning box maintaining a regeneration liquid column of 510 mm was installed in such a way that the gap between top most water surface and spinneret bottom is between 15 to 25 mm. 5 mm gap was provided in the funnel bottom portion. Regeneration liquid flow rate of 10 to 15 m3/hr was sufficient to maintain full level in spinning box. The velocity of the liquid isJcept at 190 m/min.
  • Example 2 11% cellulose Lyocell polymer solution was fed at the rate of 0.01 grams/hole/min through a rectangular spinneret having 20 rows of 80 micron diameter holes, giving an extrusion speed of 1.72 rn/min. Spinning box was maintained at regeneration liquid column of 170 mm. 4 mm gap was provided in the funnel bottom portion. Regeneration liquid flow rate of 7 m3/hr was sufficient to maintain full level in spinning box. The velocity of the liquid is kept at 109 m/min. Although the water velocity at the outlet of the funnel is much higher, the drag imparted to the filaments made them to attenuate at 8 m/min speed, thus giving a draw ratio of 4.6.
  • Web laying speed was kept at 1 to 3 m/min to obtain a uniform non-woven. Vacuum of 255 mm of water column was provided below the laying portion. Web obtained on the belt was washed clear off the solvent and sent to multi layering device and then for bonding. Different samples were prepared by varying the number of layers to get non- woven samples of different coverage. Results obtained were very similar to those disclosed above.
  • the present invention can also be worked on viscose to achieve similar comparative results.
  • Process from Viscose to Web or from Lyocell dope to Web involves only one step of drying (in the final stage after spun lacing), thus saving one complete step of drying as compared to non-woven webs made through staple fiber — carded spun laced route. This process also eliminates tow cutting, fiber opening and carding steps.
  • Process uses only continuous fibers, hence no chances of short fibers resulting into linting, ideal for producing wipes for clean room application

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nonwoven Fabrics (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)

Abstract

La présente invention concerne un procédé de préparation d'une structure cellulosique non-tissée comprenant les étapes d'extrusion de filaments continus à partir d'une solution cellulosique, d'acheminement des filaments extrudés à travers un liquide de régénération de manière à atténuer les filaments et de placement des filaments atténués dans une bande. Cette invention a aussi pour objet la structure cellulosique non-tissée ainsi préparée.
EP05823538A 2004-09-17 2005-09-16 Procede de preparation d'une structure cellulosique non- tissee et structure cellulosique non-tissee ainsi preparee Withdrawn EP1791996A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN999MU2004 2004-09-17
PCT/IN2005/000315 WO2006035458A1 (fr) 2004-09-17 2005-09-16 Procede de preparation d'une structure cellulosique non- tissee et structure cellulosique non-tissee ainsi preparee

Publications (1)

Publication Number Publication Date
EP1791996A1 true EP1791996A1 (fr) 2007-06-06

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP05823538A Withdrawn EP1791996A1 (fr) 2004-09-17 2005-09-16 Procede de preparation d'une structure cellulosique non- tissee et structure cellulosique non-tissee ainsi preparee

Country Status (6)

Country Link
US (1) US20080023873A1 (fr)
EP (1) EP1791996A1 (fr)
JP (1) JP2008513620A (fr)
KR (1) KR20070061826A (fr)
CN (1) CN101023211A (fr)
WO (1) WO2006035458A1 (fr)

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TWI621742B (zh) * 2014-11-26 2018-04-21 使用熔噴方式製備具有吸濕轉移性不織布的方法
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CN105316869B (zh) * 2015-11-25 2018-08-21 青岛大学 基于湿法纺丝技术制备纯壳聚糖纤维长丝无纺布的工艺及设备
EP3231899A1 (fr) * 2016-04-14 2017-10-18 TreeToTextile AB Procédé et système pour la production d'une composition de solution à filer
AT519489B1 (de) 2016-10-21 2021-11-15 Chemiefaser Lenzing Ag Verfahren und Vorrichtung zum Herstellen von Vliesen auf Cellulosebasis, die direkt aus Lyocell-Spinnlösung gebildet werden
US11220790B2 (en) 2017-01-20 2022-01-11 The Procter & Gamble Company Multi-ply fibrous structures
US11149383B2 (en) 2017-01-20 2021-10-19 The Procter & Gamble Company Layered fibrous structures
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US10814587B2 (en) 2018-06-04 2020-10-27 The Procter & Gamble Company Fibrous structures comprising a movable surface
US10786972B2 (en) 2018-06-04 2020-09-29 The Procter & Gamble Company Thick and absorbent and/or flexible toilet tissue
TWI827634B (zh) * 2018-07-17 2024-01-01 奧地利商蘭仁股份有限公司 用於從紡絲黏合織物之生產中的處理空氣分離溶劑之方法及裝置
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CN112981578A (zh) * 2019-12-12 2021-06-18 连津格股份公司 后处理和整理方法

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WO2006035458B1 (fr) 2006-11-02
KR20070061826A (ko) 2007-06-14
JP2008513620A (ja) 2008-05-01
WO2006035458A1 (fr) 2006-04-06
CN101023211A (zh) 2007-08-22
US20080023873A1 (en) 2008-01-31

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