WO2000058539A1 - Non tisse lace par filage de poly(alcool vinylique) - Google Patents
Non tisse lace par filage de poly(alcool vinylique) Download PDFInfo
- Publication number
- WO2000058539A1 WO2000058539A1 PCT/US2000/003918 US0003918W WO0058539A1 WO 2000058539 A1 WO2000058539 A1 WO 2000058539A1 US 0003918 W US0003918 W US 0003918W WO 0058539 A1 WO0058539 A1 WO 0058539A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- fabric
- web
- poly
- vinyl alcohol
- fibers
- 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.)
- Ceased
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
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/4309—Polyvinyl alcohol
-
- 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
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
- D04H1/43835—Mixed fibres, e.g. at least two chemically different fibres or fibre blends
Definitions
- the present invention relates to nonwoven fabrics made from poly(vinyl alcohol), and particularly to nonwoven fabrics made from poly(vinyl alcohol) by the spunlace process.
- Spunlaced fabrics are produced by carding a plurality of fabrics into a sheet, and subsequently passing the sheet under water jets to hydroentangle the fibers.
- Spunlaced fabrics are nonwoven, and thus do not require complex weaving steps or machinery for their preparation.
- Spunlaced fabrics also are different from other nonwoven fabrics, which must be thermobonded, chemically bonded, or stitchbonded, to produce a fabric of sufficient strength for commercial use.
- U.S. Patent No. 5,093,190 to Kwok et al. discloses a process for making spunlaced acrylic/polyester fabrics. Johnson & Johnson and Maxxim Medical manufacture and sell spunlaced fabrics made from polyester and cellulose fibers. The above mentioned spunlaced fabrics are feasible for many commercial applications. However, it would be desirable to improve the performance of these fabrics in a number of respects, including bursting strength, air permeability, tensile strength, flammability, absorbency, impact penetration, water vapor transmission, and water repellency.
- the invention provides a poly(vinyl alcohol) fabric produced by a method comprising the consecutive steps of supporting a plurality of poly(vinyl alcohol) fibers on a mesh screen to form a web, pressure liquid entangling the web, and drying the web.
- the invention provides a fabric comprising a poly(vinyl alcohol) fibrous web, wherein the fabric is nonwoven, binding adhesives are substantially absent from the fabric, heat fusion is substantially absent from the fabric, needlepunching is substantially absent from the fabric, and stitchbonding is substantially absent from the fabric.
- the invention provides a method of finishing a poly(vinyl alcohol) fabric to impart water repellence to the fabric comprising contacting the fabric with an aqueous finishing formulation, and subsequently drying the fabric and/or curing the finish at a temperature above the water solubility temperature of the poly(vinyl alcohol).
- the invention provides a method of making a poly(vinyl alcohol) fabric comprising (a) supporting a plurality of poly(vinyl alcohol) fibers on a mesh screen to form a web; (b) pressure liquid entangling the web; and (c) drying the web.
- X and Y are present at a weight ratio of 2:5, and are present in such ratio regardless of whether additional components are contained in the compound.
- a weight percent of a component is based on the total weight of the formulation or composition in which the component is included.
- a residue of a chemical species refers to the moiety that is the resulting product of the chemical species in a particular reaction scheme or subsequent formulation or chemical product, regardless of whether the moiety is actually obtained from the chemical species.
- an ethylene glycol residue in a polyester refers to one or more -OCH 2 CH 2 O- units in the polyester, regardless of whether ethylene glycol was used to prepare the polyester.
- a sebacic acid residue in a polyester refers to one or more -CO(CH 2 ) 8 CO- moieties in the polyester, regardless of whether the residue is obtained by reacting sebacic acid or an ester thereof to obtain the polyester.
- an effective amount of a compound or property as provided herein is meant such amount as is capable of performing the function of the compound or property for which an effective amount is expressed.
- the exact amount required will vary from process to process, depending on recognized variables such as the compounds employed and the processing conditions observed. Thus, it is not possible to specify an exact "effective amount.” However, an appropriate effective amount may be determined by one of ordinary skill in the art using only routine experimentation.
- Heat fusion refers to any method in which fibers are bonded by application of heat, and includes thermobonding.
- Pressure liquid entangling refers to a process for entangling fibers in a web of fabric by spraying a plurality of liquid jets onto the web and thereby entangling the fibers. Pressure liquid entangling thus includes hydro entangling using jets of water.
- Degree of hydrolysis also includes degree of saponification where saponification is employed in the preparation of poly(vinyl alcohol). Description of the Invention
- the invention provides a poly( vinyl alcohol) fabric produced by a method comprising the consecutive steps of (a) supporting a plurality of poly(vinyl alcohol) fibers on a mesh screen to form a web; (b) pressure liquid entangling the web; and (c) drying the web.
- the invention is preferably practiced with a poly( vinyl alcohol) and ⁇ oly(vinyl alcohol) fibers meeting the following characteristics: 1. Degree of polymerization of poly( vinyl alcohol): Preferably from about 300 to about 5000, more preferably from about 800 to about 3000, and still more preferably from about 1200 to about 2000.
- Degree ofhydrolysis ofpoly(vinyl alcohol) Preferably greater than 80%, more preferably greater than 85%, even more preferably greater than 90%, still even more preferably greater than 95%, even further preferably greater than 97%, and still even further preferably greater than 98%.
- Average denier of fibers Preferably from about 0.1 to about 10, more preferably from about 0.5 and about 5, and even more preferably from about 1 to about 3 denier.
- Average length of fibers Preferably from about 4 mm to about 300 mm, more preferably from about 20 to about 100 mm, even more preferably from about 30 to about 60 mm, and most preferably about 38 mm.
- the fibers can be cold water soluble, or soluble at room temperature, to facilitate eventual disposal.
- the pressure liquid entangling can be performed under any conditions that does not detrimentally affect the properties of the web in a substantial way.
- the liquid entangling is preferably performed with water.
- Poly( vinyl alcohol) fibers that are cold water soluble or soluble at room temperature, and which might be at least partially dissolved by hydroentangling, can be entangled by liquids which are nonexplosive, have a low boiling point, and do not readily dissolve poly(vinyl alcohol).
- the pressure liquid entangling is preferably performed at a water pressure of from about 10 to about 200 bar, more preferably at a water pressure of from about 20 to about 120 bar, and even more preferably at a water pressure of from about 40 to about 100 bar.
- the drying is preferably performed at a temperature of from about 20°C to about 230°C, more preferably from about 60°C to about 130°C, and even potentially at a temperature that exceeds the solubility temperature of the poly( vinyl alcohol).
- the drying is preferably performed by passing heated air through the web. Even more preferably, the web is dried by passing it over a perforated drum that draws air through the fabric and into the perforated drum.
- the method might also preferably comprise other steps, including, after step (a), the steps of cross-lapping the web; and stretching the web in the machine direction.
- the method might also comprise, after step (c), winding the web onto a roll.
- the web preferably satisfies the following criteria after step (c):
- Thickness Preferably from about 0.05 to about 2 mm, more preferably from about 0.1 mm to about 1 mm, still more preferably from about from about 0.3 mm to about 0.6 mm, and most preferably about 0.4 mm.
- Base weight Preferably from about 20 g/m 2 to about 400 g/m 2 , more preferably from about 35 to about 200 g/m 2 , even more preferably from about 40 to about 100 g/m 2 , still even more preferably from about 50 to about 80 g/m 2 , and most preferably about 70 g/m 2 .
- the poly(vinyl alcohol) fibers may also be carded along with other fibers selected from the group consisting of polyester, polypropylene, polyethylene, rayon, cellulose, nylon, ethyl ene/(meth)acrylic acid copolymer, and other fibrous polymers known in the art.
- the method may further comprise, after step c, adhering a substantially impermeable layer to the web.
- the layer preferably comprises poly(vinyl alcohol) polyethylene, polypropylene, polyester, ethylene/(meth)acrylic acid copolyester, or any other polymer known to form impermeable layers.
- the substantially impermeable layer can be adhered to the web by methods including extrusion coating, laminating, spraying, dipping and roll coating.
- the finished web may further comprise, and preferably be substantially saturated with, a solvent, so that the web can be used as a wipe.
- the method can further comprise, after step (c), contacting (and optionally saturating to greater than 10%, 25%, 40%, 60%, 75%, 90%, or 100% saturation) the web with a solvent liquid such as isopropyl alcohol, water, methyl ethyl ketone, methyl propyl ketone, and acetone.
- the method further comprises contacting the web with an aqueous finishing formulation to impart water repellency to the fabric, preferably before step (c).
- an aqueous finishing formulation comprises a fluorocarbon and a wax and preferably contributes from about 0.01 to about 3 wt. % fluorocarbon, and from about 0.01 to about 15 or 20 wt. % wax, to the weight of the fabric.
- the fabric preferably satisfies one or more of the following properties, and can satisfy any combination of the following properties. These properties are especially useful in fabrics that are about 0.4 mm thick, and that have a base weight of about 70 g/m 2 . It will be understood that the strength attributes given below can be extrapolated based upon increases or decreases from a 0.4 mm thick fabric having a base weight of about 70 g/m 2 . 1.
- the fabric preferably has a tensile strength in the machine direction greater than about 13 pounds, more preferably about 17 pounds, and more preferably about 20 pounds, when measured for a one inch strip according to ASTM D5035-95.
- the fabric preferably has a tensile strength in the cross direction greater than 13 pounds, more preferably about 17 pounds, and more preferably about 20 pounds, when measured for a one inch strip according to ASTM D5035-95.
- the fabric preferably has a bursting strength greater than about 50, 60, 70, or 80 psi when measured by ASTM D3776-96. 4.
- the fabric preferably has an air permeability of greater than about 100, 125, or 150 CFM/sq. ft. when measured by ASTM D737-96.
- the fabric preferably has a flammability rating of IBE or DNI when measured according to ASTM D1230-94. This flammability rating is especially useful for surgical fabrics such as gowns and drapes that are exposed to laser surgery, and which are at greater risk of flammability.
- the fabric preferably has a water impact penetration less than 1.5, 1.2, or 1.0 grams when measured by AATCC 42-94.
- the fabric preferably has cumulative linting, when measured by LNDA 1ST, of less than 7000, 5000, or 4000 in the 0.3 - lO ⁇ range, and less than 6000, 4500, or 3500 in the >0.5// range.
- the fabrics of this invention have many uses, especially in the medical industry.
- the fabric is configured into a surgical fabric, preferably selected from the group consisting of gowns, drapes, and protective apparel.
- the fabric is configured into an absorbent pad, preferably selected from the group consisting of gauze, swabs, towels, and wipes.
- the fabric is configured into an air filter.
- the fabrics of this invention preferably derive their strength from the pressure liquid entanglement of fibers within the web. This is in contrast to poly(vinyl alcohol) fabrics of the prior art, in which the fabric derived its structural integrity and strength by weaving, binding adhesives, heat fusion, needlepunching, and stitchbonding.
- fabrics of the present invention are also distinct from prior art poly(vinyl alcohol) fabrics in several other respects, including one or more of the following: (1 ) the fabric is typically not woven to any substantial degree; (2) binding adhesives are typically absent from the fabric to any substantial degree; (3) the fabric is typically not heat fused to any substantial degree; (4) the fabric is typically not needlepunched to any substantial degree; and/or (5) the fabric is typically not stitchbonded to any substantial degree.
- Substantial degree refers to a level of bonding which contributes more to the strength of the fabric than entanglement from liquid jets.
- the fabrics of this invention can also be characterized by properties other than the method of making described above.
- the invention provides a fabric in which (1) weaving is substantially absent, (2) binding adhesives are substantially absent, (3) heat fusion is substantially absent, (4) needlepunching is substantially absent, and (5) stitchbonding is substantially absent.
- This distinct embodiment represents an alternative description of the fabrics of this invention, and it will be understood that the preferred process and fabric limitations discussed above apply to this embodiment as well.
- the invention provides a method of finishing a poly( vinyl alcohol) fabric to impart water repellence to the fabric comprising contacting the fabric with an aqueous finishing formulation, and subsequently drying the fabric and/or curing the finish at a temperature above the water solubility temperature of the poly(vinyl alcohol).
- the invention provides a method of making a poly( vinyl alcohol ) fabric comprising: (a) supporting a plurality of poly(vinyl alcohol) fibers on a mesh screen to form a web; (b) pressure liquid entangling the web; and (c) drying the web.
- the following is one set of processing data to make 65 gsm sp unlace PVA fabric.
- Example 2 polyfvinyl alcohol
- Pillmg test condition 9 kpa load, abradant is plain weave cross bred and worsted wool fibers, 5,000 cycles maximum.
- Class 1 in Pilling:: very severe pilling
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Professional, Industrial, Or Sporting Protective Garments (AREA)
- Absorbent Articles And Supports Therefor (AREA)
- Materials For Medical Uses (AREA)
- Laminated Bodies (AREA)
Abstract
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000608816A JP2002540317A (ja) | 1999-03-26 | 2000-02-16 | スパンレース加工ポリ(ビニルアルコール)布 |
| AU40013/00A AU4001300A (en) | 1999-03-26 | 2000-02-16 | Spunlaced poly(vinyl alcohol) fabrics |
| EP00919305A EP1169505A1 (fr) | 1999-03-26 | 2000-02-16 | Non tisse lace par filage de poly(alcool vinylique) |
| CA002365849A CA2365849A1 (fr) | 1999-03-26 | 2000-02-16 | Non tisse lace par filage de poly(alcool vinylique) |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US28079199A | 1999-03-26 | 1999-03-26 | |
| US09/280,791 | 1999-03-26 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2000058539A1 true WO2000058539A1 (fr) | 2000-10-05 |
Family
ID=23074672
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/US2000/003918 Ceased WO2000058539A1 (fr) | 1999-03-26 | 2000-02-16 | Non tisse lace par filage de poly(alcool vinylique) |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP1169505A1 (fr) |
| JP (1) | JP2002540317A (fr) |
| CN (1) | CN1352710A (fr) |
| AU (1) | AU4001300A (fr) |
| CA (1) | CA2365849A1 (fr) |
| WO (1) | WO2000058539A1 (fr) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005007959A1 (fr) * | 2003-07-16 | 2005-01-27 | Fleissner Gmbh | Torchon entierement synthetique, procede et dispositif de realisation du torchon |
| WO2005068700A1 (fr) * | 2003-12-17 | 2005-07-28 | Kimberly-Clark Worldwide, Inc. | Produits de nettoyage pre-satures hydrodispersibles |
| WO2010123480A1 (fr) * | 2009-04-23 | 2010-10-28 | Precision Fabrics Group, Inc. | Serviettes chirurgicales générant moins de particules de peluche |
| EP2734665A4 (fr) * | 2011-07-18 | 2015-08-19 | Lakeland Ind Inc | Nouveaux articles à base d'alcool polyvinylique |
| US9797073B1 (en) | 2011-07-18 | 2017-10-24 | Lakeland Industries, Inc. | Process for producing polyvinyl alcohol articles |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5191811B2 (ja) * | 2008-06-05 | 2013-05-08 | ユニチカ株式会社 | ビニロン短繊維を含むスパンレース不織布の製造方法 |
| CN106998986B (zh) * | 2014-12-22 | 2019-07-05 | 花王株式会社 | 清扫用片材 |
| CN118407191B (zh) * | 2024-06-27 | 2024-09-03 | 浙江理工大学 | 一种核防护用可水溶水刺非织造材料及其加工方法和应用 |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1060102A (en) * | 1963-05-23 | 1967-02-22 | Geigy Ag J R | Treatment of textile fibres |
| FR1555705A (fr) * | 1966-11-14 | 1969-01-31 | ||
| US4570311A (en) * | 1981-12-07 | 1986-02-18 | Firma Carl Freudenberg | Method for manufacturing water soluble fabric for chemical laces |
| US4731277A (en) * | 1985-08-08 | 1988-03-15 | Firma Carl Freudenberg | Nonwoven textile sponge for medicine and hygiene, and methods for the production thereof |
| EP0491383A1 (fr) * | 1990-12-19 | 1992-06-24 | Mitsubishi Paper Mills, Ltd. | Non-tissé et son procédé de réalisation |
| US5500068A (en) * | 1994-02-23 | 1996-03-19 | International Paper Company | Absorbent, flushable, bio-degradable, medically-safe nonwoven fabric with PVA binding fibers, and process for making the same |
| JPH08311757A (ja) * | 1995-05-15 | 1996-11-26 | Kuraray Co Ltd | 耐水性ポリビニルアルコール系繊維からなる不織布シート |
| DE19620503A1 (de) * | 1996-05-22 | 1997-11-27 | Fleissner Maschf Gmbh Co | Verfahren zur Herstellung eines Vlieses durch hydromechanisches Vernadeln und Produkt nach diesem Herstellungsverfahren |
| WO1998010126A1 (fr) * | 1996-09-09 | 1998-03-12 | Isolyser Company, Inc. | Procede de mise au rebut de vetements solubles dans l'eau chaude et de tissus analogues |
-
2000
- 2000-02-16 AU AU40013/00A patent/AU4001300A/en not_active Abandoned
- 2000-02-16 CA CA002365849A patent/CA2365849A1/fr not_active Abandoned
- 2000-02-16 EP EP00919305A patent/EP1169505A1/fr not_active Withdrawn
- 2000-02-16 WO PCT/US2000/003918 patent/WO2000058539A1/fr not_active Ceased
- 2000-02-16 CN CN00808060A patent/CN1352710A/zh active Pending
- 2000-02-16 JP JP2000608816A patent/JP2002540317A/ja active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1060102A (en) * | 1963-05-23 | 1967-02-22 | Geigy Ag J R | Treatment of textile fibres |
| FR1555705A (fr) * | 1966-11-14 | 1969-01-31 | ||
| US4570311A (en) * | 1981-12-07 | 1986-02-18 | Firma Carl Freudenberg | Method for manufacturing water soluble fabric for chemical laces |
| US4731277A (en) * | 1985-08-08 | 1988-03-15 | Firma Carl Freudenberg | Nonwoven textile sponge for medicine and hygiene, and methods for the production thereof |
| EP0491383A1 (fr) * | 1990-12-19 | 1992-06-24 | Mitsubishi Paper Mills, Ltd. | Non-tissé et son procédé de réalisation |
| US5500068A (en) * | 1994-02-23 | 1996-03-19 | International Paper Company | Absorbent, flushable, bio-degradable, medically-safe nonwoven fabric with PVA binding fibers, and process for making the same |
| JPH08311757A (ja) * | 1995-05-15 | 1996-11-26 | Kuraray Co Ltd | 耐水性ポリビニルアルコール系繊維からなる不織布シート |
| DE19620503A1 (de) * | 1996-05-22 | 1997-11-27 | Fleissner Maschf Gmbh Co | Verfahren zur Herstellung eines Vlieses durch hydromechanisches Vernadeln und Produkt nach diesem Herstellungsverfahren |
| WO1998010126A1 (fr) * | 1996-09-09 | 1998-03-12 | Isolyser Company, Inc. | Procede de mise au rebut de vetements solubles dans l'eau chaude et de tissus analogues |
Non-Patent Citations (1)
| Title |
|---|
| PATENT ABSTRACTS OF JAPAN vol. 1997, no. 03 31 March 1997 (1997-03-31) * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005007959A1 (fr) * | 2003-07-16 | 2005-01-27 | Fleissner Gmbh | Torchon entierement synthetique, procede et dispositif de realisation du torchon |
| WO2005068700A1 (fr) * | 2003-12-17 | 2005-07-28 | Kimberly-Clark Worldwide, Inc. | Produits de nettoyage pre-satures hydrodispersibles |
| US7378360B2 (en) | 2003-12-17 | 2008-05-27 | Kimberly-Clark Worldwide, Inc. | Water dispersible, pre-saturated wiping products |
| US9913762B2 (en) | 2008-04-28 | 2018-03-13 | Precision Fabrics Group, Inc. | Surgical towels with reduced lint particle generation |
| WO2010123480A1 (fr) * | 2009-04-23 | 2010-10-28 | Precision Fabrics Group, Inc. | Serviettes chirurgicales générant moins de particules de peluche |
| EP2734665A4 (fr) * | 2011-07-18 | 2015-08-19 | Lakeland Ind Inc | Nouveaux articles à base d'alcool polyvinylique |
| US9523172B2 (en) | 2011-07-18 | 2016-12-20 | Lakeland Industries, Inc. | Process for producing polyvinyl alcohol articles |
| US9797073B1 (en) | 2011-07-18 | 2017-10-24 | Lakeland Industries, Inc. | Process for producing polyvinyl alcohol articles |
| US11168441B2 (en) | 2011-07-18 | 2021-11-09 | Lakeland Industries, Inc. | Process for producing polyvinyl alcohol articles |
Also Published As
| Publication number | Publication date |
|---|---|
| CA2365849A1 (fr) | 2000-10-05 |
| CN1352710A (zh) | 2002-06-05 |
| AU4001300A (en) | 2000-10-16 |
| EP1169505A1 (fr) | 2002-01-09 |
| JP2002540317A (ja) | 2002-11-26 |
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