CA2054277C - Cardable hydrophobic polyolefin fiber, material and method for preparation thereof - Google Patents
Cardable hydrophobic polyolefin fiber, material and method for preparation thereofInfo
- Publication number
- CA2054277C CA2054277C CA002054277A CA2054277A CA2054277C CA 2054277 C CA2054277 C CA 2054277C CA 002054277 A CA002054277 A CA 002054277A CA 2054277 A CA2054277 A CA 2054277A CA 2054277 C CA2054277 C CA 2054277C
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- Canada
- Prior art keywords
- fibre
- filament
- spin
- phosphoric acid
- acid ester
- 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.)
- Expired - Fee Related
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Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
-
- 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
- D04H1/4291—Olefin 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
- 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
- D04H1/4391—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 characterised by the shape of the fibres
- D04H1/43918—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 characterised by the shape of the fibres nonlinear fibres, e.g. crimped or coiled fibres
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M7/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made of other substances with subsequent freeing of the treated goods from the treating medium, e.g. swelling, e.g. polyolefins
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/40—Reduced friction resistance, lubricant properties; Sizing compositions
-
- 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
- Y10T428/2909—Nonlinear [e.g., crimped, coiled, etc.]
-
- 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
- Y10T428/2922—Nonlinear [e.g., crimped, coiled, etc.]
-
- 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
- Y10T428/2933—Coated or with bond, impregnation or core
-
- 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
- Y10T428/2933—Coated or with bond, impregnation or core
- Y10T428/2962—Silane, silicone or siloxane in coating
-
- 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
- Y10T428/2933—Coated or with bond, impregnation or core
- Y10T428/2964—Artificial fiber or filament
- Y10T428/2967—Synthetic resin or polymer
-
- 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.]
- Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
- Y10T442/603—Including strand or fiber material precoated with other than free metal or alloy
- Y10T442/607—Strand or fiber material is synthetic polymer
Abstract
An improved method for producing hydrophobic polyolefin-containing staple fiber for processing, with reduced waste and improved crimp by sequential treatment with two finish compositions comprising at least one neutralized phosphoric acid ester and at least one polysiloxane of defined classes and amounts.
Description
20a4277 _ This invention relates to a process using topically applied fiber finishes to obtain polyolefin-containing hydrophobic fiber or filament capable of accepting a high crimp without undue end waste in subsequent processing operations and without substantial loss of hydrophobicity in the resulting fiber or nonwoven product.
A particularly troublesome technical problem arises when a high degree of hydrophobicity is desired on cuffs or borders in a diaper or similar product produced from conventionally-bonded webs of hydrophobic fiber such as polyolefin-containing staple. This problem arises because the untreated hydrophobic fiber quickly becomes unworkable due to friction and accumulated static charges generated during conventional processing such as spinning, crimping, cutting and carding. For this reason, the prior art recognizes the use of various topically-applied fiber lubricants and finishes which generally change fiber surface properties sufficiently to permit processing. Unfortunately, however, such conventional treatment often results in fibers and nonwoven end products which are substantially more hydrophilic than desired and difficult to control quality-wise. In particular, because of the nature of commercial high speed fiber-processing operations, and the unpredictable affinity of known finishing agents to individual batches or bales of hydrophobic fiber, it becomes very difficult (a) to obtain a full crimp in the fiber component and to maintain a uniform hydrophobicity in the final nonwoven product.
-The above identified desirable properties may be obtained, according to the present invention, by treatment of a continuous spun polyolefin fibre or filament with a finish composed of up to 100% polysiloxane. Such a treatment, known as spin finishing, is desirably in an amount of about 0.09% to 0.5%, based on the weight of the fibre.
After spin finishing the fibre may be crimped and then, to facilitate further processing, the fibre is, in a preferred embodiment of the present invention, treated with a composition composed of up to 100% of a neutralized phosphoric acid ester.
Such a treatment of a spin-finished crimped fibre is referred to herein as over finishing. An effective amount of over finish will desirably be in the range of 0.05% to 0.80%, based on the weight of the fibre.
According to the present invention, the spin finish composition may contain an amount of neutralized phosphoric acid ester, in addition to a polysiloxane. Such phosphoric acid ester component in the spin finish composition is desirably present in an amount of from about 5% to about 50% of the spin finish.
A suitable polysiloxane for use in the process of the present invention is represented by the formula:
S-(Si-O)o-Y
wherein X and Y are individually defined as a hydrophobic chemical end group such as a lower alkyl group, R' is individually defined as a lower alkyl such as a methyl group, and 0 is defined as a positive number within the range of about 10-50 or higher.
An appropriate neutralized phosphoric acid ester for use in the process of the present invention may be represented by the formula:
o (Alk-O) n~P~O~R~
wherein X and Y are individually defined as a hydrophobic chemical end group such as a lower alkyl group, R' is individually defined as a lower alkyl such as a methyl group, and O is defined as a positive number within the range of about 10-50 or higher.
As desired, the above-obtained fibre is formed into webs, compiled and bonded in a conventional manner to obtain a desired hydrophobic nonwoven material.
In a broad aspect, therefore, it will be understood that the present invention relates to a substantially hydrophobic fibre comprising: (i) a spun polyolefin filament; and (ii) a polysiloxane spin finish on the surface of said filament.
In another broad aspect, the present invention relates to a method for preparing polyolefin-containing high crimp spin fibre or filament suitable for production of nonwoven material of high hydrophobicity, comprising:
A. initially treating corresponding continuous spin fibre or filament with an effective amount of a first modifier finish comprising, comprising (a) 0% to about 70% by weight of modifier composition of at least one neutralized phosphoric acid ester represented by the formula:
O (1) Il (Alk-O)n-P-O-R~
~ - 3(a) - 2054277 wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not S less than about 1, the sum of which is about 3; and (b) about 100%-30% by weight of first modifier composition of at least one polysiloxane represented by the formula:
R' (2) X--(Si--O)o~Y
R' wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher;
B. crimping the resulting treated continuous fibre or filament;
C. applying to the continuous fibre or filament, at a point downstream of the crimping step, an effective amount of a second modifier composition comprising (a) about 100%-5% by weight of second modifier composition, of at least one neutralized phosphoric acid ester represented by formula (l); and (b) 0% to about 95% by weight of second modifier composition, comprising at least one polysiloxane represented by formula (2) in sufficient amount to obtain a final cumulative concentration on the fibre within a range of about .01%-1.0% based on fibre weight;
D. processing the resulting modifier-treated fibre or filament.
A
A particularly troublesome technical problem arises when a high degree of hydrophobicity is desired on cuffs or borders in a diaper or similar product produced from conventionally-bonded webs of hydrophobic fiber such as polyolefin-containing staple. This problem arises because the untreated hydrophobic fiber quickly becomes unworkable due to friction and accumulated static charges generated during conventional processing such as spinning, crimping, cutting and carding. For this reason, the prior art recognizes the use of various topically-applied fiber lubricants and finishes which generally change fiber surface properties sufficiently to permit processing. Unfortunately, however, such conventional treatment often results in fibers and nonwoven end products which are substantially more hydrophilic than desired and difficult to control quality-wise. In particular, because of the nature of commercial high speed fiber-processing operations, and the unpredictable affinity of known finishing agents to individual batches or bales of hydrophobic fiber, it becomes very difficult (a) to obtain a full crimp in the fiber component and to maintain a uniform hydrophobicity in the final nonwoven product.
-The above identified desirable properties may be obtained, according to the present invention, by treatment of a continuous spun polyolefin fibre or filament with a finish composed of up to 100% polysiloxane. Such a treatment, known as spin finishing, is desirably in an amount of about 0.09% to 0.5%, based on the weight of the fibre.
After spin finishing the fibre may be crimped and then, to facilitate further processing, the fibre is, in a preferred embodiment of the present invention, treated with a composition composed of up to 100% of a neutralized phosphoric acid ester.
Such a treatment of a spin-finished crimped fibre is referred to herein as over finishing. An effective amount of over finish will desirably be in the range of 0.05% to 0.80%, based on the weight of the fibre.
According to the present invention, the spin finish composition may contain an amount of neutralized phosphoric acid ester, in addition to a polysiloxane. Such phosphoric acid ester component in the spin finish composition is desirably present in an amount of from about 5% to about 50% of the spin finish.
A suitable polysiloxane for use in the process of the present invention is represented by the formula:
S-(Si-O)o-Y
wherein X and Y are individually defined as a hydrophobic chemical end group such as a lower alkyl group, R' is individually defined as a lower alkyl such as a methyl group, and 0 is defined as a positive number within the range of about 10-50 or higher.
An appropriate neutralized phosphoric acid ester for use in the process of the present invention may be represented by the formula:
o (Alk-O) n~P~O~R~
wherein X and Y are individually defined as a hydrophobic chemical end group such as a lower alkyl group, R' is individually defined as a lower alkyl such as a methyl group, and O is defined as a positive number within the range of about 10-50 or higher.
As desired, the above-obtained fibre is formed into webs, compiled and bonded in a conventional manner to obtain a desired hydrophobic nonwoven material.
In a broad aspect, therefore, it will be understood that the present invention relates to a substantially hydrophobic fibre comprising: (i) a spun polyolefin filament; and (ii) a polysiloxane spin finish on the surface of said filament.
In another broad aspect, the present invention relates to a method for preparing polyolefin-containing high crimp spin fibre or filament suitable for production of nonwoven material of high hydrophobicity, comprising:
A. initially treating corresponding continuous spin fibre or filament with an effective amount of a first modifier finish comprising, comprising (a) 0% to about 70% by weight of modifier composition of at least one neutralized phosphoric acid ester represented by the formula:
O (1) Il (Alk-O)n-P-O-R~
~ - 3(a) - 2054277 wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not S less than about 1, the sum of which is about 3; and (b) about 100%-30% by weight of first modifier composition of at least one polysiloxane represented by the formula:
R' (2) X--(Si--O)o~Y
R' wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher;
B. crimping the resulting treated continuous fibre or filament;
C. applying to the continuous fibre or filament, at a point downstream of the crimping step, an effective amount of a second modifier composition comprising (a) about 100%-5% by weight of second modifier composition, of at least one neutralized phosphoric acid ester represented by formula (l); and (b) 0% to about 95% by weight of second modifier composition, comprising at least one polysiloxane represented by formula (2) in sufficient amount to obtain a final cumulative concentration on the fibre within a range of about .01%-1.0% based on fibre weight;
D. processing the resulting modifier-treated fibre or filament.
A
- 3(b) - 205~277 In yet another broad aspect, the present invention relates to a method of preparing polyolefin containing high crimp spin fibre or filament for production of nonwoven material exhibiting hydrophobicity, and in particular to the improvement comprising applying to the surface of a continuous spun fibre or filament, a modifier comprising:
R' X- ( si-o ) o~Y
wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher.
For present purposes, the term "polyolefin-containing spun fibre or filament" is defined as including continuous as well as staple melt spun fibres obtainable from conventionally blended isotactic polypropylene as well as hydrophobic copolymers thereof with ethylene, l-butene, 4-methylpentene-1 and the like.
The resulting blended and extruded spun melt conveniently has a weight average varying from about 3 X 105 to about 5 X 105, a molecular weight distribution of about 2.0-12.0, a metal flow rate of about 5-70 g/10 minutes, and a spin temperature conveniently within a range of about 220 C-325 C.
Also includible within spun melt of the present process are art-recognized fibre additives, including pH stabilizers such as calcium stearate, antioxidants, pigments, including whiteners and colorants such as Tio2 and the like. Generally, such additives vary from about .05%-3% by weight of spun melt.
~' 205~2~r7 The present invention i8 found particularly applicable to high æpeed production of a variety of nonwoven materials utilizing webs obtained, for instance, from carded staple and may also comprise additional web components such as fibrillated film and the like.
The term "processing~ as used herein in process step ~D~, includes art-recognized web formation techniques applied to continuous as well as crimped, cut and carded staple fiber, the crimping step, being optional with respect to webs formed solely of fiber or filament.
Continuous spun fiber or filaments used to form webs within the present invention preferably comprise topically treated spun melt staple fiber, filament, or fibrillated film of bicomponent or monofilament types, the modifier compositions or finishes being conventionally applied, for instance, by drawing over a feed wheel partially immersed in a bath of modifier composition, dipped therein, or by spraying, in effective amounts to permit fiber processing, and then dried.
For present purposes, webs used to form nonwovens within the scope of the present invention can be formed by spun bonded, melt blown or conventional "Dry" carded Process using staple fiber and then bonded together using techniques employing adhesive binders (USP 4,535,013), calender rolls, hot air, sonic, laser, pressure bonding, needle punching and the like, known to the art.
Webs used to fabricate nonwoven material can also usefully comprise conventional sheath/core (concentric or otherwise) or side-by-side bicomponent fiber or filament, alone or combined with treated or untreated homogenous-type fiber or filament and/or fibrillated film.
Also within the scope of the present invention is the use of nonwovens comprised of one or more bonded webs of modifier-treated polyolefin fiber- and/or fiber-like (fibrillated film) components having a mixed fiber denier of homogeneous and/or bicomponent types not exceeding about 40 dpf. Such webs preferably utilize fiber or filaments within a range of about 0.1-40 dpf.
_ _ 5 2~5~277 Webs used in forming nonwovens within the scope of the present invention are produced from one or more types of con-ventionally spun fibres or filaments having, for instance, round, delta, trilobal, or diamond cross sectional configurations, or mixtures thereof.
Nonwoven cover stock of the above-defined types can usefully vary in weight from about 10 - 45 gm yd2 or higher.
The invention is further illustrated but not limited by the following Example and Tables:
A. Polypropylene fibre samples S-1 and S-2 are separately spun from separate resin batches in flake form generally characterized as follows:
a crystallinity 60%, a molecular weight distribution 6.4 a melt flow 3.2 g/10 minutes which are individually processed in an impact blender. After 30 minutes the individual mixes having MFR values within a range of 24-27, are separately spun through a 210 circular hole spin-nerette at 280 C. The resulting spun filaments, are air quenched at room temperature, and stretched at 115 C. (4X) to obtain 2.0-2.54 dpf circular filaments, to which spin and over finishes are applied upstream and downstream of a conventional steam crimper by passing the filaments over a feed or kiss wheel partly immersed in a first modifier finish composition consisting of LurolR AS-Y and LE458HS polysiloxane emulsion (5%/95% by wt), LurolR AS-Y being a neutralized phosphoric acid/alcohol ester product of George A. Goulston Company of Monroe, NC, and LE 45 BHS being a polydimethylsiloxane product of Union Carbide Corporation. Contact is of sufficient duration to apply about .40% and .59% dried spin composition (based on tow weight). The coated continuous filaments are then individually batch crimped at 100 C and then passed over a second kiss roll at sufficient speed and concentration to coat the fibre with an over finish consisting of 100% Lurol AS-Y to impart .1% over finish to the dry fibre.
~' 2~5~277 After air drying, the coated and processed test fiber is chopped to 1.5" length staple and set aside for conventional tests. Test results are summarized and reported in Table I
below, in which the relative retained hydrophobicity as determined by fiber contact angle (% of fiber having a contact angle greater than 90o) of the processed fiber is indicated in column 3 and the relative amounts of spinned finish (first modifier) an over finish (second modifier) are set out in columns 5 and 6 and by footnote.
B. Polypropylene samples S-3 through S-6 obtained from a resin batch essentially as described in Example l-A are spun, air ~uenched and crimped as described therein, using different spin finish (first modifier) and over finish (second modifier) compositions identically applied by using a Kiss roll to impart from .1%-.5% (dry fiber weight) of spin finish and 0%-.10% (dry fiber weight) over finish to obtain a total residual finish (after crimp) of about .2%-.3% by weight. The crimping conditions are kept constant as an example in A. The observed waste (i.e. residue left on spool) and imparted crimp is also recorded in Table 2 below.
-~ I
ST~D!-F pp~PFTTl~C
s . Percent by *2 *3 Color Degree of *1 Weight rinish Fiber Tenacity Elongation Spin Fin. Over Fin.
n sa~c~_L Tyge ~ydro~AbiCitY ~ (*T5o) S~ yle ~ U ~ ~ Cpi Iyve/~MT Type/~MT
S-l 195 5 26.8 0.4 0.3 2.0 2.10 236.6 34.1 262/0.6 263/0.1 S-2 195 5 24.4 0.59 0.25 2.07 2.72 226.1 25.2 262/0.6 263/0.1 *1 Relative hydrophobicity of the finished and processed fiber; 1 substantially hydrophilic, 5 . substantially hydrophobic.
*2 Finish ~262: 95~ Polydi~ethylsilo~ane Enulsion (LE45B~S) 5~ Lurol AS~
*3 Finish ~263 100~ Lurol ASY
-8- 20~277 ._ o o ~ o .
.~
.~ ~ ~ ~o o o o _ o o o o ~
g g e~
o o ~o ~o .
_ Z ~0 r W
~, ~ r~
, U~
.
o o o o P~
o o o ~ ~ ~ o ~o ~o m m ~ -c ~ ~ ~ 3 ~ ~ z o~ ~ ~o ~o o ~
~ ~ a I I I I
V~
O ~ O
~, 20~4277 g C. Polypropylene resin samples corresponding to those identified as samples S-3 and S-6 in Example lB and Table II
are routinely tested to determine differences in percent hydrophobicity obtained in the processed and finished fiber utilizing different spin finish (step one) and over finish (step two) based on fiber contact angle determinations.
(Wilhelmy; The Physical Chemistry of Surfaces; 3rd Ed. Wiley Sons, 1976; page 344). Test results are reported in Table 3 below.
20542~7 _ TABLE III
FIBER AVG. a RANGE OF a% HYDROPHOBICITY
R' X- ( si-o ) o~Y
wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher.
For present purposes, the term "polyolefin-containing spun fibre or filament" is defined as including continuous as well as staple melt spun fibres obtainable from conventionally blended isotactic polypropylene as well as hydrophobic copolymers thereof with ethylene, l-butene, 4-methylpentene-1 and the like.
The resulting blended and extruded spun melt conveniently has a weight average varying from about 3 X 105 to about 5 X 105, a molecular weight distribution of about 2.0-12.0, a metal flow rate of about 5-70 g/10 minutes, and a spin temperature conveniently within a range of about 220 C-325 C.
Also includible within spun melt of the present process are art-recognized fibre additives, including pH stabilizers such as calcium stearate, antioxidants, pigments, including whiteners and colorants such as Tio2 and the like. Generally, such additives vary from about .05%-3% by weight of spun melt.
~' 205~2~r7 The present invention i8 found particularly applicable to high æpeed production of a variety of nonwoven materials utilizing webs obtained, for instance, from carded staple and may also comprise additional web components such as fibrillated film and the like.
The term "processing~ as used herein in process step ~D~, includes art-recognized web formation techniques applied to continuous as well as crimped, cut and carded staple fiber, the crimping step, being optional with respect to webs formed solely of fiber or filament.
Continuous spun fiber or filaments used to form webs within the present invention preferably comprise topically treated spun melt staple fiber, filament, or fibrillated film of bicomponent or monofilament types, the modifier compositions or finishes being conventionally applied, for instance, by drawing over a feed wheel partially immersed in a bath of modifier composition, dipped therein, or by spraying, in effective amounts to permit fiber processing, and then dried.
For present purposes, webs used to form nonwovens within the scope of the present invention can be formed by spun bonded, melt blown or conventional "Dry" carded Process using staple fiber and then bonded together using techniques employing adhesive binders (USP 4,535,013), calender rolls, hot air, sonic, laser, pressure bonding, needle punching and the like, known to the art.
Webs used to fabricate nonwoven material can also usefully comprise conventional sheath/core (concentric or otherwise) or side-by-side bicomponent fiber or filament, alone or combined with treated or untreated homogenous-type fiber or filament and/or fibrillated film.
Also within the scope of the present invention is the use of nonwovens comprised of one or more bonded webs of modifier-treated polyolefin fiber- and/or fiber-like (fibrillated film) components having a mixed fiber denier of homogeneous and/or bicomponent types not exceeding about 40 dpf. Such webs preferably utilize fiber or filaments within a range of about 0.1-40 dpf.
_ _ 5 2~5~277 Webs used in forming nonwovens within the scope of the present invention are produced from one or more types of con-ventionally spun fibres or filaments having, for instance, round, delta, trilobal, or diamond cross sectional configurations, or mixtures thereof.
Nonwoven cover stock of the above-defined types can usefully vary in weight from about 10 - 45 gm yd2 or higher.
The invention is further illustrated but not limited by the following Example and Tables:
A. Polypropylene fibre samples S-1 and S-2 are separately spun from separate resin batches in flake form generally characterized as follows:
a crystallinity 60%, a molecular weight distribution 6.4 a melt flow 3.2 g/10 minutes which are individually processed in an impact blender. After 30 minutes the individual mixes having MFR values within a range of 24-27, are separately spun through a 210 circular hole spin-nerette at 280 C. The resulting spun filaments, are air quenched at room temperature, and stretched at 115 C. (4X) to obtain 2.0-2.54 dpf circular filaments, to which spin and over finishes are applied upstream and downstream of a conventional steam crimper by passing the filaments over a feed or kiss wheel partly immersed in a first modifier finish composition consisting of LurolR AS-Y and LE458HS polysiloxane emulsion (5%/95% by wt), LurolR AS-Y being a neutralized phosphoric acid/alcohol ester product of George A. Goulston Company of Monroe, NC, and LE 45 BHS being a polydimethylsiloxane product of Union Carbide Corporation. Contact is of sufficient duration to apply about .40% and .59% dried spin composition (based on tow weight). The coated continuous filaments are then individually batch crimped at 100 C and then passed over a second kiss roll at sufficient speed and concentration to coat the fibre with an over finish consisting of 100% Lurol AS-Y to impart .1% over finish to the dry fibre.
~' 2~5~277 After air drying, the coated and processed test fiber is chopped to 1.5" length staple and set aside for conventional tests. Test results are summarized and reported in Table I
below, in which the relative retained hydrophobicity as determined by fiber contact angle (% of fiber having a contact angle greater than 90o) of the processed fiber is indicated in column 3 and the relative amounts of spinned finish (first modifier) an over finish (second modifier) are set out in columns 5 and 6 and by footnote.
B. Polypropylene samples S-3 through S-6 obtained from a resin batch essentially as described in Example l-A are spun, air ~uenched and crimped as described therein, using different spin finish (first modifier) and over finish (second modifier) compositions identically applied by using a Kiss roll to impart from .1%-.5% (dry fiber weight) of spin finish and 0%-.10% (dry fiber weight) over finish to obtain a total residual finish (after crimp) of about .2%-.3% by weight. The crimping conditions are kept constant as an example in A. The observed waste (i.e. residue left on spool) and imparted crimp is also recorded in Table 2 below.
-~ I
ST~D!-F pp~PFTTl~C
s . Percent by *2 *3 Color Degree of *1 Weight rinish Fiber Tenacity Elongation Spin Fin. Over Fin.
n sa~c~_L Tyge ~ydro~AbiCitY ~ (*T5o) S~ yle ~ U ~ ~ Cpi Iyve/~MT Type/~MT
S-l 195 5 26.8 0.4 0.3 2.0 2.10 236.6 34.1 262/0.6 263/0.1 S-2 195 5 24.4 0.59 0.25 2.07 2.72 226.1 25.2 262/0.6 263/0.1 *1 Relative hydrophobicity of the finished and processed fiber; 1 substantially hydrophilic, 5 . substantially hydrophobic.
*2 Finish ~262: 95~ Polydi~ethylsilo~ane Enulsion (LE45B~S) 5~ Lurol AS~
*3 Finish ~263 100~ Lurol ASY
-8- 20~277 ._ o o ~ o .
.~
.~ ~ ~ ~o o o o _ o o o o ~
g g e~
o o ~o ~o .
_ Z ~0 r W
~, ~ r~
, U~
.
o o o o P~
o o o ~ ~ ~ o ~o ~o m m ~ -c ~ ~ ~ 3 ~ ~ z o~ ~ ~o ~o o ~
~ ~ a I I I I
V~
O ~ O
~, 20~4277 g C. Polypropylene resin samples corresponding to those identified as samples S-3 and S-6 in Example lB and Table II
are routinely tested to determine differences in percent hydrophobicity obtained in the processed and finished fiber utilizing different spin finish (step one) and over finish (step two) based on fiber contact angle determinations.
(Wilhelmy; The Physical Chemistry of Surfaces; 3rd Ed. Wiley Sons, 1976; page 344). Test results are reported in Table 3 below.
20542~7 _ TABLE III
FIBER AVG. a RANGE OF a% HYDROPHOBICITY
Claims (28)
OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A substantially hydrophobic fibre comprising:
i) a spun polyolefin filament; and ii) a polysiloxane spin finish on the surface of said filament.
i) a spun polyolefin filament; and ii) a polysiloxane spin finish on the surface of said filament.
2. A fibre as claimed in Claim 1, wherein said polysiloxane spin finish is a polysiloxane represented by the formula wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher.
3. A fibre or filament as claimed in Claim 2, wherein said filament has applied thereto an over finish including a neutralized phosphoric acid ester.
4. A fibre or filament as claimed in Claim 3, wherein said neutralized phosphoric acid ester has the following formula:
wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not less than about 1, the sum of which is about 3.
wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not less than about 1, the sum of which is about 3.
5. A fibre or filament as claimed in Claim 4, wherein said over finish further includes polysiloxane.
6. A fibre or filament as claimed in Claim 5, wherein said polysiloxane has the formula:
wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher.
wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher.
7. A fibre or filament as claimed in Claim 1, wherein in said over finish, said neutralized phosphoric acid ester and said polysiloxane are present in amounts of 100% - 5% neutralized phosphoric acid ester and 0% - 95% polysiloxane.
8. A fibre or filament as claimed in any one of Claims 1 - 7, wherein said spin finish on said filament includes a neutralized phosphoric acid ester component.
9. A fibre or filament as claimed in any one of Claims 1 - 7, wherein said spin finish on said filament includes a neutralized phosphoric acid ester component, in an amount of from 0% to 40%, relative to the content of said polysiloxane in said spin finish, and said neutralized phosphoric acid ester is represented by the formula:
wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not less than about 1, the sum of which is about 3.
wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not less than about 1, the sum of which is about 3.
10. A fibre or filament as claimed in any one of Claims 1 - 7, wherein said spin finish on said filament includes a neutralized phosphoric acid ester component, in an amount of from 0% to 40%, relative to the content of said polysiloxane in said spin finish, and said neutralized phosphoric acid ester is represented by the formula:
wherein (Alk-O) represents a straight 1-4 carbon alkoxy group, R is defined as an amino group or an alkali metal, n is 2, and m is 1.
wherein (Alk-O) represents a straight 1-4 carbon alkoxy group, R is defined as an amino group or an alkali metal, n is 2, and m is 1.
11. A fibre or filament as claimed in any one of Claims 1 - 7, wherein said fibre or filament is composed of polypropylene.
12. A fibre or filament as claimed in Claim 8, wherein said fibre is a polypropylene fibre having a spin finish of from 0.1%
to 0.5% by weight.
to 0.5% by weight.
13. A fibre or filament as claimed in Claim 9, wherein said fibre is a polypropylene fibre having a spin finish of from 0.1%
to 0.5% by weight.
to 0.5% by weight.
14. A fibre or filament as claimed in Claim 10, wherein said fibre is a polypropylene fibre having a spin finish of from 0.1%
to 0.5% by weight.
to 0.5% by weight.
15. A fibre or filament as claimed in Claim 12, 13 or 14, wherein said fibre is crimped.
16. A method for preparing polyolefin-containing high crimp spin fibre or filament suitable for production of nonwoven material of high hydrophobicity, comprising:
A. initially treating corresponding continuous spin fibre or filament with an effective amount of a first modifier finish comprising, comprising (a) 0% to about 70% by weight of modifier composition of at least one neutralized phosphoric acid ester represented by the formula:
(1) (1) wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not less than about 1, the sum of which is about 3; and (b) about 100%-30% by weight of first modifier composition of at least one polysiloxane represented by the formula:
(2) wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher;
B. crimping the resulting treated continuous fibre or filament;
C. applying to the continuous fibre or filament, at a point downstream of the crimping step, an effective amount of a second modifier composition comprising (a) about 100%-5% by weight of second modifier composition, of at least one neutralized phosphoric acid ester represented by formula (1); and (b) 0% to about 95% by weight of second modifier composition, comprising at least one polysiloxane represented by formula (2) in sufficient amount to obtain a final cumulative concentration on the fibre within a range of about .01%-1.0% based on fibre weight;
D. processing the resulting modifier-treated fibre or filament.
A. initially treating corresponding continuous spin fibre or filament with an effective amount of a first modifier finish comprising, comprising (a) 0% to about 70% by weight of modifier composition of at least one neutralized phosphoric acid ester represented by the formula:
(1) (1) wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not less than about 1, the sum of which is about 3; and (b) about 100%-30% by weight of first modifier composition of at least one polysiloxane represented by the formula:
(2) wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher;
B. crimping the resulting treated continuous fibre or filament;
C. applying to the continuous fibre or filament, at a point downstream of the crimping step, an effective amount of a second modifier composition comprising (a) about 100%-5% by weight of second modifier composition, of at least one neutralized phosphoric acid ester represented by formula (1); and (b) 0% to about 95% by weight of second modifier composition, comprising at least one polysiloxane represented by formula (2) in sufficient amount to obtain a final cumulative concentration on the fibre within a range of about .01%-1.0% based on fibre weight;
D. processing the resulting modifier-treated fibre or filament.
17. The method of Claim 16, wherein the Alk-0 group of the neutralized phosphoric acid ester is defined as a straight 1-4 carbon alkoxy group; n is 2; and m is 1.
18. The method of Claim 16, wherein at least some of the second modifier composition is topically applied to fibre or filament upstream of the crimping step.
19. The method of Claim 16, wherein the second modifier composition is topically applied to an at least partially crimped continuous spin fibre or filament.
20. The method of Claim 16, wherein the "D" processing step comprises a fibre cutting and carding operation.
21. The method of Claim 16, wherein the second modifier composition comprises 0-15% by weight of a polysiloxane represented by the formula (2).
22. A polyolefin-containing spin fibre or filament obtained in accordance with the method of Claim 16.
23. A polyolefin-containing spin fibre or filament obtained in accordance with the method of Claim 17.
24. A polyolefin-containing spin fibre or filament obtained in accordance with the method of Claim 20.
25. A nonwoven material obtained by compiling and bonding the polyolefin-containing spin fibre or filament as processed in Claim 24.
26. In a method of preparing polyolefin containing high crimp spin fibre or filament for production of nonwoven material exhibiting hydrophobicity, the improvement comprising applying to the surface of a continuous spun fibre or filament, a modifier comprising:
wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher.
wherein X and Y are individually defined as a hydrophobic chemical end group, R' is individually defined as a lower alkyl group, and o is defined as a positive number within the range of about 10-50 or higher.
27. The improved method of Claim 26, further comprising treating said fibre or filament with a neutralized phosphoric acid ester.
28. The improved method of Claim 27, wherein said neutralized phosphoric acid ester has the formula:
wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not less than about 1, the sum of which is about 3.
wherein Alk is individually defined as a lower alkyl group, R is defined as an amino group or an alkali metal, n and m are individually defined as positive numbers of not less than about 1, the sum of which is about 3.
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EP (1) | EP0486158B1 (en) |
JP (1) | JPH04289234A (en) |
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- 1991-10-16 SG SG1996005272A patent/SG49022A1/en unknown
- 1991-10-16 DE DE91309511T patent/DE486158T1/en active Pending
- 1991-10-16 DK DK91309511.3T patent/DK0486158T3/en active
- 1991-10-16 EP EP91309511A patent/EP0486158B1/en not_active Expired - Lifetime
- 1991-10-16 AT AT91309511T patent/ATE139276T1/en active
- 1991-10-16 ES ES91309511T patent/ES2087976T3/en not_active Expired - Lifetime
- 1991-10-25 CA CA002054277A patent/CA2054277C/en not_active Expired - Fee Related
- 1991-10-30 FI FI915120A patent/FI915120A/en unknown
- 1991-11-08 MX MX9101989A patent/MX9101989A/en unknown
- 1991-11-11 TW TW080108885A patent/TW253919B/zh active
- 1991-11-13 IL IL10004491A patent/IL100044A/en not_active IP Right Cessation
- 1991-11-14 JP JP3299193A patent/JPH04289234A/en active Pending
- 1991-11-14 BR BR919104961A patent/BR9104961A/en not_active Application Discontinuation
- 1991-11-14 NO NO914465A patent/NO304194B1/en unknown
- 1991-11-14 KR KR1019910020246A patent/KR920010047A/en not_active Application Discontinuation
- 1991-11-14 AU AU87889/91A patent/AU647841B2/en not_active Ceased
-
1994
- 1994-03-30 US US08/220,465 patent/US5721048A/en not_active Expired - Lifetime
-
1996
- 1996-06-27 GR GR960401726T patent/GR3020357T3/en unknown
- 1996-08-01 HK HK148196A patent/HK148196A/en not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
EP0486158A2 (en) | 1992-05-20 |
DE69120209T2 (en) | 1996-10-24 |
EP0486158B1 (en) | 1996-06-12 |
ATE139276T1 (en) | 1996-06-15 |
IL100044A0 (en) | 1992-08-18 |
NO914465D0 (en) | 1991-11-14 |
AU8788991A (en) | 1992-05-21 |
EP0486158A3 (en) | 1992-07-08 |
MX9101989A (en) | 1992-07-08 |
CA2054277A1 (en) | 1992-05-16 |
NO304194B1 (en) | 1998-11-09 |
AU647841B2 (en) | 1994-03-31 |
NO914465L (en) | 1992-05-18 |
GR3020357T3 (en) | 1996-09-30 |
DE69120209D1 (en) | 1996-07-18 |
KR920010047A (en) | 1992-06-26 |
FI915120A0 (en) | 1991-10-30 |
HK148196A (en) | 1996-08-09 |
TW253919B (en) | 1995-08-11 |
JPH04289234A (en) | 1992-10-14 |
BR9104961A (en) | 1992-06-23 |
ES2087976T3 (en) | 1996-08-01 |
SG49022A1 (en) | 1998-05-18 |
US5721048A (en) | 1998-02-24 |
FI915120A (en) | 1992-05-16 |
DE486158T1 (en) | 1993-12-16 |
IL100044A (en) | 1994-10-21 |
DK0486158T3 (en) | 1996-10-21 |
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Legal Events
Date | Code | Title | Description |
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EEER | Examination request | ||
MKLA | Lapsed | ||
MKLA | Lapsed |
Effective date: 20001025 |