CA1298695C - Elasticized non-woven fabric and method of making the same - Google Patents
Elasticized non-woven fabric and method of making the sameInfo
- Publication number
- CA1298695C CA1298695C CA000499301A CA499301A CA1298695C CA 1298695 C CA1298695 C CA 1298695C CA 000499301 A CA000499301 A CA 000499301A CA 499301 A CA499301 A CA 499301A CA 1298695 C CA1298695 C CA 1298695C
- Authority
- CA
- Canada
- Prior art keywords
- fibers
- elasticizable
- web
- textile
- percent
- 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 - Lifetime
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
-
- 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
- D04H1/04—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres having existing or potential cohesive properties, e.g. natural fibres, prestretched or fibrillated artificial fibres
- D04H1/08—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres having existing or potential cohesive properties, e.g. natural fibres, prestretched or fibrillated artificial fibres and hardened by felting; Felts or felted products
- D04H1/16—Laminated felts in which the separate layers are united by a felting process
-
- 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
- D04H1/4326—Condensation or reaction polymers
- D04H1/4358—Polyurethanes
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nonwoven Fabrics (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
- Woven Fabrics (AREA)
- Treatment Of Fiber Materials (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
An elasticized non-woven fiber material is made by combining one or more textile fibers with one or more elas-ticizeable fibers and bonding the combined fibers together.
The resultant web of bonded non-woven fibers is then heat-treated to heat-shrink the elasticizeable fiber and recover its elasticity thereby shrinking the fibers and the web of material. An elasticized non-woven fabric made by the de-scribed method is also provided.
An elasticized non-woven fiber material is made by combining one or more textile fibers with one or more elas-ticizeable fibers and bonding the combined fibers together.
The resultant web of bonded non-woven fibers is then heat-treated to heat-shrink the elasticizeable fiber and recover its elasticity thereby shrinking the fibers and the web of material. An elasticized non-woven fabric made by the de-scribed method is also provided.
Description
~2~ 33S
Field Of The_Invention The present invention concerns non-woven fiber materi-als, in particular elasticized non-woven fiber materials and a method of making such materials.
Description Of Related Art The manufacture of elasticized non-woven ~iber materi-als by the technique of combining conventional texile fibers with elasticizeable fibers and heat-treating the fabric to elasticize the elasticizeable fibers is shown in U.S. Patent 4,426,420 (Likhyani). This patent discloses the preparation 15 of non-woven batts comprising a so-called "hard fiber" and "potentially elastic" fiber. The hard fibers are described as comprising any synthetic or natural fiber forming materi-~ al such as polyesters, polyamides, etc., or natural fibers ;~ such as cotton, silk,~paper, etc. The potentially elastic fibers are stated to be elastomeric compositions of the type which are elasticized by heat-treatment. The Likhyani pat-ent discloses a method for making a so-called "spunlaced"
non-woven fabric wherein a batt composed of at least two types of staple fibers is sub jected to hydraulic entangle-ment by fine, high pressure columnar streams of water whichentangle the fibers to provide the spunlaced material. Af-ter the entanglement, the resultant fabric is heat-treated to develop elastic characteristics in the elastomeric fi-bers. The elastomeric filaments are extruded, cold-drawn and cut to desired fiber length as described in the sole ex-ample of the patent.
SUMMARY OF THE INVENTION
; 35 In accordance with the present invention there is provided a method for making a non-woven elasticized fiber ' ~ ~ .
: ~.
.
material which comprises combinin~, blending or inte~ 9 at least one type of textile fiber with at least one ty~:~e o~
uniaxially oriented elasticizeable fiber, bonding the com-bined fibers to each other to form a web, matrix, sheet or the like, and heating the resultant web to heat-shrin~ the oriented fiber which thereby resumes or recovers its elastic properties. The resultant web thereby exhibits elastomeric properties.
One aspect of the invention includes combining about l~ to 50%, preferably 5~ to 35~, by weigh~ of the elasti-cizeable fiber with about 99% to 50~, preferably 95~ to 65~, by weight of the textile fiber.
In another aspect of the invention the elasticizeable fiber comprises an extruded synthetic elastomeric polymer, and the method includes the steps of cold-drawing an elas-ticizeable filament to uniaxially orient the filament to stretch it by at least about 100~, preferably about 100% to 500~, of its initial len~th, then cutting to preform fila-ments to a desired fiber length. This fiber is combined with, and bonded to, the textile fiber while the elasticized fiber is in its oriented condition to form a suitable web.
In accordance with the invention, the resultant web is heat-shrunk, preferably at a temperature of about 7~C to 200C, to shrink the oriented fiber to about 10~ to 90% of z5 its elongated length.
Another aspect of the invention includes combining at least one type of textile fiber, at least one type of melt blown fiber and at least one type of elasticizeable fiber to form the fiber material web. In certain aspects of the in-vention the elasticizeable fiber is selected from the group ;~ consisting o s~yrene-butadiene copolymers, styrene-butadi-ene-styrene copolymers and polyurethane.
In accordance with the invention, there is also pro-vided an elasticized non-woven fiber material comprising at least one type of textile fiber bonded to at least one type of elastic fiber obtained by heat-treatment of an oriented preform, the tex~ile fiber being retracted and pleated upon .
.
LZ98&i95 heat-shrinking of the preform to elasticize the elastLc ~i-ber but the textile iber being sufficiently ~ree to extend to about its original tension level upon being stretched.
The ~iber material may further include at least one type of melt blown ~iber.
DESCRIPTION OF THE PREFERE~ED EMBODIMENTS
Non-woven fabrics are of course well known in the art and generally comprise ~ex~ile fibers, which may be of vary-ing length from very short fibers to very long or substanti-ally continuous fibers, which have been combined to form a web or batt of non-woven fabric. As used herein and in the claims the term "textile fiber~ is intended to broadly in-clude any fiber which is useful in making a non-woven fa-bric. Such fibers may be made of synthetic organic polymer-ic materials, processed natural materials or a combination thereof. By way of illustration and without limitation, synthetic polymeric fibers which are useful as textile fi-bers in the present invention include polyester fibers,polyamide fibers such as nylon, acrylic ~olymer and copoly-mer fibers, glass fibers, polyolefin fibers such as polyeth-ylene and polypropylene fibers, cellulosic derivatives such as rayon, and combined fibers such as fibers of one material sheathed with a casing of another material. For example, ; polypropylene fibers sheathed with polyethylene are known in the art. Fibers made from processed natural materials, i.e., natural fibers, which are useful as textile fibers in the present invention include, without limitation, cotton, silk, wool, pulp or paper and the like as well as blends or combinations of any two or more of the foregoing fibers.
Such textile fibers are usually distinguished in the art from elastic fibers as the textile fibers generally have extremely limited elasticity characteristics. That is, they 35 usually would elongate no more than 40%, usually 20~ to 40~
of their initial length before breaking and generally have a modulus of elasticity in the range of about 18 to 85 grams , . .
298~9S
per denier, but may be higher.
As used herein and in the claims, the ter~ "elasti-cizeable Eiber" has reference to those materials, usually synthetic polymeric elastomeric materials, which (a) can be extruded into filaments, (b) be drawn, usually at ambient temperature ~cold-drawn) to elongate, stretch or orient the filaments, which will retain ~heir stretched condition upon being relaxed by release of the drawing tension, and (c) upon bein~ heated to an elevated temperature the tensioned material will markedly shrink and thereby recover or resume its elastomeric property. By being "elasticized" it is meant that the heat-shrunk ibers will be able to be stretched to all or nearly all of their relaxed, pre-heated elongated length and return to approximately their heat-lS shrunk length upon release of the stretching force.Preferably, the stretched filament is cut to desired fiber length, which length will depend upon such factors as the particular process employed or the end use of the material.
Prior to elasticization, the elasticizeable fibers can be air-laid, carded or otherwise formed into non-woven webs in ; substantially the same manner as textile fibers.
By "cold-drawing" as used herein and in the claims is meant the technique of drawing or stretching the elastomeric - filament or preform when it has cooled to substantially be-~- 25 low its extrusion temperature, usually when it has cooled to ambient temperature. Such drawing is conventionally utiliz-ed to strengthen and reduce the diameter of the extruded fi-ber. The cold-drawing as utilized in the present invention is carried out at a temperature below the extrusion tempera-ture, pre~erably at ambient temperature, and the cold-draw-ing is preferably carried out to an extent to elongate the fiber by about 100% to 500~ or more, e.g., 1,000%, but usu-; ally about 100% to 400% of its initial length.
In the prac~ice of the present invention, the elasti-cizeable fiber is combined with the ~extile fiber, and mayoptionally be combined with other materials such as melt blown fibers, by any suitable technique such as dry-laid, 29~369~
wet-laid or carding techniques and the combined ~i~ers are then bonded by any suitable technique which will not heat the elongated elasticizeable fibers so as to shrink them since, in accordance with the invention, heat-shrinking o~
S the elasticizeable fibers is carried ou~ after they are bonded to the textile fibers or the textile and melt blown fibers. Thus, adhesive, e.g., latex spray bonding, sonic wave bonding, or any combination of suitable techniques may be employed, so long as the elasticizeable fiber shrinking temperatures are avoided until the bonding operation is car-ried out. The result is a shrinkable, that is, a heat-shrinkable, fiber material in which the shrinking of the elasticizeable fibers will shrink the web of bonded elasti-cizeable and textile fibers. A preferred method o~ bonding is to spray a light coating of any suitable adhesive, such as a latex, e.g., a urethane latex, onto the web of combined fibers. ~he fibers may be combined in any suitable way and, as used herein and in the claims, the term "adhesive" is ; used broadly to mean any material which will bond the com-bined fibers one ~o the other and is otherwise suitable for ~; the purposes of the invention. The adhesive or sonic bond-ing is preferred as it physically joins the fibers, not merely by frictional entanglement, so that the heat-treat-~ ment to shrink and thereby elasticize the elasticizeable fi-; ~5 ber relaxes the textile fibers so that they do not impede stretching of the elasticized fibers. The web of fiber ma-terial after heat-treatment will be reduced in its length and width dimensions.
After the combined fibers are bonded together, the re-sultant fiber material web is heated by any suitable means such as being passed through an oven, under heating lamps, infra red radiation, or the like, in order to heat the elas-ticizeable fibers sufficiently to shrink them to impart the desired elastic characteristics thereto. The fiber material containing the elasticizeable fibers is in a relaxed condi-tion during the heating step to allow contraction.
A significant advantaqe provided by the technique of ., , ~9~gs the invention is that inasmuch as the elasticizeable ~ ~ers are oriented when they are bonded to the textile ~ibe~s, upon shrinking o~ the fo~mer the textile ~ibers bonced thereto will retract and loop or pleat as the elasticizea~le ibers contract. Consequently, when the finished fabric is stretched, even if it is stretched to a degree which returns the now elasticized fibers to their original pre-shrunk length, there is sufficient play in the textile ~ibers that they do not restrain stretching o~ the fabric. In other words, maximum stretching o the elas~icized ~ibers, even to their pre-shrunk length, will extend the textile fibers only to the tension level they were at when they were bonded to the unshrunken elasticizeable fibers. This contributes greatly to the comfort and stretchability of the non-woven fabric o~ the invention.
The elasticizeable fibers useful in the invention may be any suitable fiber, as described above. One elasticize-able fiber ~ound to be useful is sold under the trademark KRATON by Shell Chemical Company and another is sold under the trademark ESTANE by B. F. ~x~-ich Company Other suit-able compositions are those disclosed in U.S. Patents 3,007,227, 3,651,014, 3,766,143, and 3,7b3,109.
; The ESTANE elasticizeable fiber is a urethane poly-mer and the KRATON elasticizeable fiber is a styrene-butadi-ene~styrene copolymer.
The following examples illustrate specific embodi-ments of the invention.
Examole 1 Several grades of urethane elasticizeable polymers sold under the trademark ESTANE by .B. F. ~x~rich C~ny and several grades of styrene-butadiene-styrene elasticize-able polymer sold under the tradema~k ~RATON byShell Chemlcal Ccmpany were extruded into ~ilaments. The ex~ruder had ~our heat zones along the screw, typically maintained at re-spective temperatures of 148.9C, 168.3C, 176.7C and ~, ,: . . .
l~g~
182.2C in the direction oE extrusion. The die comprised eight openings of 10 mil diameter each and a die pressure oE
from 3,500 to 5,500 psi was utilized. After cooling to am-bient temperature, the extruded filaments were cold-drawn over rollers with the following typical results, dependent on specific ex~rusion conditions:
TABL~ I
:
10 Elasticizeable Polymer ~a) ~b) (c) (d) ESTANE 5707 8,000 122.110.616 308 ESTANE 5710 7,000 135.180.341 254 RRATON 1102 4,600 390.30.19a 1085 KRATON 3200 1,700 139.80.076 268 ~, (a~ ~ Nominal tensile strength Psr (b) = Denier per filament (c) = Tensile strength, grams per denier (d) = ~ elongation to breakage .~
The percentage elongations to breakage show highly elastic fibers which, after heat treatment, are shrinkable to a fraction of their elongated length and elastic between ap-proximately their heat-shrunk and elongated lengths.
`:
Example 2 A four-ply supercrimp nylon fiber was Eormed into a 30 carded web and stretched, elasticizeable Eibers made of KRATON 3200 copolymer extruded as described above were air-laid onto the carded nylon. The elasticizeable fibers had a denier o 139.8, 0.076 grams per denier and an elongation to breakage of 268%. The fiber content of the finished web 35 comprised 60% by weight elasticizeable fiber and 40~ by weight nylon. Upon heating, the web of fiber material show-ed shrinkage and corresponding elasticity as Eollows:
~Z9~36~5 Heating Temperature ~ Shrinkage o~ Web_ Sample 80C 120 C150C
`~ 1 29 3S 44 3 2g 33 43 :
Example 3 A bonded web was prepared from 1.5 parts by weight Enka Rayon 700 1 9/16 inch staple fibers, l.S parts by weight 1 9/16 inch polypropylene staple fibers and 12 parts by weight KRATON 3200 elasticizeable fiber of Example 2. A
urethane binder li~uid was sprayed onto the web in a pattern of nearly touching 1/8 inch diameter dots by use of a spray template. The urethane binder comprised 80~ by weight of the finished bonded web. Upon heating at 120-130C, the web of fiber material sustained 38~ shrinkage.
A bonded web was prepared from ~ parts by weight polypropylene 1 9/16 inch staple fibers, 9 parts by weight KRATON 3200 fibers per Example 2 cut to 1 9/16 inch staple length, and the combined fibers were bonded with a pattern of five dots of urethane binder so that the finished web comprised 70% by weight urethane binder. Upon heating to 120-130C, the web of fiber material showed a shrinkage of 65~o The fiber webs of the invention show excellent elas ; ticity as stretchability unhampered by the limited stretch-ability of the textile fibers. This follows from the above-described method of bonding the elasticizeable fibers in their elongated, pre-shrunk state to the textile fibers in a shrinkable web.
While the invention has been described in detail with `~ respect to specific preferred embodiments thereof it will be appreciated that upon a reading and understanding of the oregoing variations and modifications to the preferred em-bodiments will occur to those skilled in the art and such variations and modifications are believed to fall within the :~ .
.
.
: - ':
-- ~2~8~i~S
spirit and scope ot the .n ~ntion and the appended cldims.
:
:`~
Field Of The_Invention The present invention concerns non-woven fiber materi-als, in particular elasticized non-woven fiber materials and a method of making such materials.
Description Of Related Art The manufacture of elasticized non-woven ~iber materi-als by the technique of combining conventional texile fibers with elasticizeable fibers and heat-treating the fabric to elasticize the elasticizeable fibers is shown in U.S. Patent 4,426,420 (Likhyani). This patent discloses the preparation 15 of non-woven batts comprising a so-called "hard fiber" and "potentially elastic" fiber. The hard fibers are described as comprising any synthetic or natural fiber forming materi-~ al such as polyesters, polyamides, etc., or natural fibers ;~ such as cotton, silk,~paper, etc. The potentially elastic fibers are stated to be elastomeric compositions of the type which are elasticized by heat-treatment. The Likhyani pat-ent discloses a method for making a so-called "spunlaced"
non-woven fabric wherein a batt composed of at least two types of staple fibers is sub jected to hydraulic entangle-ment by fine, high pressure columnar streams of water whichentangle the fibers to provide the spunlaced material. Af-ter the entanglement, the resultant fabric is heat-treated to develop elastic characteristics in the elastomeric fi-bers. The elastomeric filaments are extruded, cold-drawn and cut to desired fiber length as described in the sole ex-ample of the patent.
SUMMARY OF THE INVENTION
; 35 In accordance with the present invention there is provided a method for making a non-woven elasticized fiber ' ~ ~ .
: ~.
.
material which comprises combinin~, blending or inte~ 9 at least one type of textile fiber with at least one ty~:~e o~
uniaxially oriented elasticizeable fiber, bonding the com-bined fibers to each other to form a web, matrix, sheet or the like, and heating the resultant web to heat-shrin~ the oriented fiber which thereby resumes or recovers its elastic properties. The resultant web thereby exhibits elastomeric properties.
One aspect of the invention includes combining about l~ to 50%, preferably 5~ to 35~, by weigh~ of the elasti-cizeable fiber with about 99% to 50~, preferably 95~ to 65~, by weight of the textile fiber.
In another aspect of the invention the elasticizeable fiber comprises an extruded synthetic elastomeric polymer, and the method includes the steps of cold-drawing an elas-ticizeable filament to uniaxially orient the filament to stretch it by at least about 100~, preferably about 100% to 500~, of its initial len~th, then cutting to preform fila-ments to a desired fiber length. This fiber is combined with, and bonded to, the textile fiber while the elasticized fiber is in its oriented condition to form a suitable web.
In accordance with the invention, the resultant web is heat-shrunk, preferably at a temperature of about 7~C to 200C, to shrink the oriented fiber to about 10~ to 90% of z5 its elongated length.
Another aspect of the invention includes combining at least one type of textile fiber, at least one type of melt blown fiber and at least one type of elasticizeable fiber to form the fiber material web. In certain aspects of the in-vention the elasticizeable fiber is selected from the group ;~ consisting o s~yrene-butadiene copolymers, styrene-butadi-ene-styrene copolymers and polyurethane.
In accordance with the invention, there is also pro-vided an elasticized non-woven fiber material comprising at least one type of textile fiber bonded to at least one type of elastic fiber obtained by heat-treatment of an oriented preform, the tex~ile fiber being retracted and pleated upon .
.
LZ98&i95 heat-shrinking of the preform to elasticize the elastLc ~i-ber but the textile iber being sufficiently ~ree to extend to about its original tension level upon being stretched.
The ~iber material may further include at least one type of melt blown ~iber.
DESCRIPTION OF THE PREFERE~ED EMBODIMENTS
Non-woven fabrics are of course well known in the art and generally comprise ~ex~ile fibers, which may be of vary-ing length from very short fibers to very long or substanti-ally continuous fibers, which have been combined to form a web or batt of non-woven fabric. As used herein and in the claims the term "textile fiber~ is intended to broadly in-clude any fiber which is useful in making a non-woven fa-bric. Such fibers may be made of synthetic organic polymer-ic materials, processed natural materials or a combination thereof. By way of illustration and without limitation, synthetic polymeric fibers which are useful as textile fi-bers in the present invention include polyester fibers,polyamide fibers such as nylon, acrylic ~olymer and copoly-mer fibers, glass fibers, polyolefin fibers such as polyeth-ylene and polypropylene fibers, cellulosic derivatives such as rayon, and combined fibers such as fibers of one material sheathed with a casing of another material. For example, ; polypropylene fibers sheathed with polyethylene are known in the art. Fibers made from processed natural materials, i.e., natural fibers, which are useful as textile fibers in the present invention include, without limitation, cotton, silk, wool, pulp or paper and the like as well as blends or combinations of any two or more of the foregoing fibers.
Such textile fibers are usually distinguished in the art from elastic fibers as the textile fibers generally have extremely limited elasticity characteristics. That is, they 35 usually would elongate no more than 40%, usually 20~ to 40~
of their initial length before breaking and generally have a modulus of elasticity in the range of about 18 to 85 grams , . .
298~9S
per denier, but may be higher.
As used herein and in the claims, the ter~ "elasti-cizeable Eiber" has reference to those materials, usually synthetic polymeric elastomeric materials, which (a) can be extruded into filaments, (b) be drawn, usually at ambient temperature ~cold-drawn) to elongate, stretch or orient the filaments, which will retain ~heir stretched condition upon being relaxed by release of the drawing tension, and (c) upon bein~ heated to an elevated temperature the tensioned material will markedly shrink and thereby recover or resume its elastomeric property. By being "elasticized" it is meant that the heat-shrunk ibers will be able to be stretched to all or nearly all of their relaxed, pre-heated elongated length and return to approximately their heat-lS shrunk length upon release of the stretching force.Preferably, the stretched filament is cut to desired fiber length, which length will depend upon such factors as the particular process employed or the end use of the material.
Prior to elasticization, the elasticizeable fibers can be air-laid, carded or otherwise formed into non-woven webs in ; substantially the same manner as textile fibers.
By "cold-drawing" as used herein and in the claims is meant the technique of drawing or stretching the elastomeric - filament or preform when it has cooled to substantially be-~- 25 low its extrusion temperature, usually when it has cooled to ambient temperature. Such drawing is conventionally utiliz-ed to strengthen and reduce the diameter of the extruded fi-ber. The cold-drawing as utilized in the present invention is carried out at a temperature below the extrusion tempera-ture, pre~erably at ambient temperature, and the cold-draw-ing is preferably carried out to an extent to elongate the fiber by about 100% to 500~ or more, e.g., 1,000%, but usu-; ally about 100% to 400% of its initial length.
In the prac~ice of the present invention, the elasti-cizeable fiber is combined with the ~extile fiber, and mayoptionally be combined with other materials such as melt blown fibers, by any suitable technique such as dry-laid, 29~369~
wet-laid or carding techniques and the combined ~i~ers are then bonded by any suitable technique which will not heat the elongated elasticizeable fibers so as to shrink them since, in accordance with the invention, heat-shrinking o~
S the elasticizeable fibers is carried ou~ after they are bonded to the textile fibers or the textile and melt blown fibers. Thus, adhesive, e.g., latex spray bonding, sonic wave bonding, or any combination of suitable techniques may be employed, so long as the elasticizeable fiber shrinking temperatures are avoided until the bonding operation is car-ried out. The result is a shrinkable, that is, a heat-shrinkable, fiber material in which the shrinking of the elasticizeable fibers will shrink the web of bonded elasti-cizeable and textile fibers. A preferred method o~ bonding is to spray a light coating of any suitable adhesive, such as a latex, e.g., a urethane latex, onto the web of combined fibers. ~he fibers may be combined in any suitable way and, as used herein and in the claims, the term "adhesive" is ; used broadly to mean any material which will bond the com-bined fibers one ~o the other and is otherwise suitable for ~; the purposes of the invention. The adhesive or sonic bond-ing is preferred as it physically joins the fibers, not merely by frictional entanglement, so that the heat-treat-~ ment to shrink and thereby elasticize the elasticizeable fi-; ~5 ber relaxes the textile fibers so that they do not impede stretching of the elasticized fibers. The web of fiber ma-terial after heat-treatment will be reduced in its length and width dimensions.
After the combined fibers are bonded together, the re-sultant fiber material web is heated by any suitable means such as being passed through an oven, under heating lamps, infra red radiation, or the like, in order to heat the elas-ticizeable fibers sufficiently to shrink them to impart the desired elastic characteristics thereto. The fiber material containing the elasticizeable fibers is in a relaxed condi-tion during the heating step to allow contraction.
A significant advantaqe provided by the technique of ., , ~9~gs the invention is that inasmuch as the elasticizeable ~ ~ers are oriented when they are bonded to the textile ~ibe~s, upon shrinking o~ the fo~mer the textile ~ibers bonced thereto will retract and loop or pleat as the elasticizea~le ibers contract. Consequently, when the finished fabric is stretched, even if it is stretched to a degree which returns the now elasticized fibers to their original pre-shrunk length, there is sufficient play in the textile ~ibers that they do not restrain stretching o~ the fabric. In other words, maximum stretching o the elas~icized ~ibers, even to their pre-shrunk length, will extend the textile fibers only to the tension level they were at when they were bonded to the unshrunken elasticizeable fibers. This contributes greatly to the comfort and stretchability of the non-woven fabric o~ the invention.
The elasticizeable fibers useful in the invention may be any suitable fiber, as described above. One elasticize-able fiber ~ound to be useful is sold under the trademark KRATON by Shell Chemical Company and another is sold under the trademark ESTANE by B. F. ~x~-ich Company Other suit-able compositions are those disclosed in U.S. Patents 3,007,227, 3,651,014, 3,766,143, and 3,7b3,109.
; The ESTANE elasticizeable fiber is a urethane poly-mer and the KRATON elasticizeable fiber is a styrene-butadi-ene~styrene copolymer.
The following examples illustrate specific embodi-ments of the invention.
Examole 1 Several grades of urethane elasticizeable polymers sold under the trademark ESTANE by .B. F. ~x~rich C~ny and several grades of styrene-butadiene-styrene elasticize-able polymer sold under the tradema~k ~RATON byShell Chemlcal Ccmpany were extruded into ~ilaments. The ex~ruder had ~our heat zones along the screw, typically maintained at re-spective temperatures of 148.9C, 168.3C, 176.7C and ~, ,: . . .
l~g~
182.2C in the direction oE extrusion. The die comprised eight openings of 10 mil diameter each and a die pressure oE
from 3,500 to 5,500 psi was utilized. After cooling to am-bient temperature, the extruded filaments were cold-drawn over rollers with the following typical results, dependent on specific ex~rusion conditions:
TABL~ I
:
10 Elasticizeable Polymer ~a) ~b) (c) (d) ESTANE 5707 8,000 122.110.616 308 ESTANE 5710 7,000 135.180.341 254 RRATON 1102 4,600 390.30.19a 1085 KRATON 3200 1,700 139.80.076 268 ~, (a~ ~ Nominal tensile strength Psr (b) = Denier per filament (c) = Tensile strength, grams per denier (d) = ~ elongation to breakage .~
The percentage elongations to breakage show highly elastic fibers which, after heat treatment, are shrinkable to a fraction of their elongated length and elastic between ap-proximately their heat-shrunk and elongated lengths.
`:
Example 2 A four-ply supercrimp nylon fiber was Eormed into a 30 carded web and stretched, elasticizeable Eibers made of KRATON 3200 copolymer extruded as described above were air-laid onto the carded nylon. The elasticizeable fibers had a denier o 139.8, 0.076 grams per denier and an elongation to breakage of 268%. The fiber content of the finished web 35 comprised 60% by weight elasticizeable fiber and 40~ by weight nylon. Upon heating, the web of fiber material show-ed shrinkage and corresponding elasticity as Eollows:
~Z9~36~5 Heating Temperature ~ Shrinkage o~ Web_ Sample 80C 120 C150C
`~ 1 29 3S 44 3 2g 33 43 :
Example 3 A bonded web was prepared from 1.5 parts by weight Enka Rayon 700 1 9/16 inch staple fibers, l.S parts by weight 1 9/16 inch polypropylene staple fibers and 12 parts by weight KRATON 3200 elasticizeable fiber of Example 2. A
urethane binder li~uid was sprayed onto the web in a pattern of nearly touching 1/8 inch diameter dots by use of a spray template. The urethane binder comprised 80~ by weight of the finished bonded web. Upon heating at 120-130C, the web of fiber material sustained 38~ shrinkage.
A bonded web was prepared from ~ parts by weight polypropylene 1 9/16 inch staple fibers, 9 parts by weight KRATON 3200 fibers per Example 2 cut to 1 9/16 inch staple length, and the combined fibers were bonded with a pattern of five dots of urethane binder so that the finished web comprised 70% by weight urethane binder. Upon heating to 120-130C, the web of fiber material showed a shrinkage of 65~o The fiber webs of the invention show excellent elas ; ticity as stretchability unhampered by the limited stretch-ability of the textile fibers. This follows from the above-described method of bonding the elasticizeable fibers in their elongated, pre-shrunk state to the textile fibers in a shrinkable web.
While the invention has been described in detail with `~ respect to specific preferred embodiments thereof it will be appreciated that upon a reading and understanding of the oregoing variations and modifications to the preferred em-bodiments will occur to those skilled in the art and such variations and modifications are believed to fall within the :~ .
.
.
: - ':
-- ~2~8~i~S
spirit and scope ot the .n ~ntion and the appended cldims.
:
:`~
Claims (33)
1. A method for making an elastomeric fibrous non-woven web comprising the steps of:
combining a plurality of at least one type of a textile fiber with a plurality of at least one type of an uniaxially oriented elasticizable fiber;
bonding at least some of the textile fibers to at least some of the elasticizable fibers to form a web; and heating the web to shrink and elasticize the elasticizable fibers.
combining a plurality of at least one type of a textile fiber with a plurality of at least one type of an uniaxially oriented elasticizable fiber;
bonding at least some of the textile fibers to at least some of the elasticizable fibers to form a web; and heating the web to shrink and elasticize the elasticizable fibers.
2. The method according to claim 1, wherein the combining step is carried out so that the web comprises from about 1 percent to about 50 percent, by weight, of the elasticizable fiber and from about 99 percent to about 50 percent, by weight, of the textile fiber.
3. The method according to claim 2, wherein the combining step is carried out so that the web comprises from about 5 percent to about 35 percent, by weight, of the elasticizable fiber and from about 95 percent to about 65 percent, by weight, of the textile fiber.
4. A method for making an elastomeric non-woven web comprising the steps of:
extruding a synthetic elastomeric polymer as an elasticizable filament;
uniaxially orienting the elasticizable filament by stretching the filament by at least about 100 percent;
cutting the uniaxially oriented filament to provide a plurality of uniaxially oriented fibers;
combining a plurality of said uniaxially oriented fibers with a plurality of at least one type of textile fiber;
bonding at least some of the textile fibers to at least some of the elasticizable fibers to form a non-woven web; and heating the non-woven web to shrink and elasticize the elasticizable fibers.
extruding a synthetic elastomeric polymer as an elasticizable filament;
uniaxially orienting the elasticizable filament by stretching the filament by at least about 100 percent;
cutting the uniaxially oriented filament to provide a plurality of uniaxially oriented fibers;
combining a plurality of said uniaxially oriented fibers with a plurality of at least one type of textile fiber;
bonding at least some of the textile fibers to at least some of the elasticizable fibers to form a non-woven web; and heating the non-woven web to shrink and elasticize the elasticizable fibers.
5. The method according to claim 4, wherein the textile fibers are bonded to the elasticizable fibers by applying an adhesive thereto.
6. The method according to claim 1, wherein at least one type of melt blown fiber is combined with the textile fibers and the uniaxially oriented elasticizable fibers.
7. The method according to claim 1, wherein the heating step comprises heating the web to a temperature of from about 75 degrees Centigrade to about 200 degrees Centigrade.
8. The method according to claim 1, wherein a discreet article is formed from the web prior to the web being heated to shrink and elasticize the elasticizable fibers.
9. The method according to claim 1, wherein the elasticizable fibers are formed from a material selected from the group consisting of styrene-butadiene copolymers, styrene-butadiene styrene copolymers and polyurethanes.
10. An elastomeric non-woven web comprising:
a plurality of textile fibers which are gathered and pleated;
and a plurality of heat shrunk elasticized fibers combined with said textile fibers with at least some of the elasticized fibers being bonded to at least some of the textile fibers; and wherein the gathers and pleats of the textile fibers were formed by shrinkage of the heat shrunk elasticized fibers.
a plurality of textile fibers which are gathered and pleated;
and a plurality of heat shrunk elasticized fibers combined with said textile fibers with at least some of the elasticized fibers being bonded to at least some of the textile fibers; and wherein the gathers and pleats of the textile fibers were formed by shrinkage of the heat shrunk elasticized fibers.
11. The web according to claim 10, which further includes a plurality of melt blown fibers.
12. A method for making an elastomeric fibrous non-woven web comprising the steps of:
extruding a synthetic elastomeric polymer as an elasticizable filament;
cold-drawing the elasticizable filament to uniaxially orient the filament;
cutting the uniaxially oriented filament to provide a plurality of uniaxially oriented elasticizable fibers;
combining said plurality of uniaxially oriented elasticizable fibers with a plurality of textile fibers;
bonding at least some of the textile fibers to at least some of the elasticizable fibers to form a non-woven web; and heating the non-woven web to shrink and elasticize the elasticizable fibers.
extruding a synthetic elastomeric polymer as an elasticizable filament;
cold-drawing the elasticizable filament to uniaxially orient the filament;
cutting the uniaxially oriented filament to provide a plurality of uniaxially oriented elasticizable fibers;
combining said plurality of uniaxially oriented elasticizable fibers with a plurality of textile fibers;
bonding at least some of the textile fibers to at least some of the elasticizable fibers to form a non-woven web; and heating the non-woven web to shrink and elasticize the elasticizable fibers.
13. A method for making an elastomeric non-woven web comprising the steps of:
combining a plurality of textile fibers with a plurality of uniaxially oriented elasticizable fibers;
bonding at least some of the textile fibers to at least some of the elasticizable fibers to form a non-woven web; and heating the non-woven web to shrink and elasticize the elasticizable fibers whereby at least some of the textile fibers are gathered and pleated.
combining a plurality of textile fibers with a plurality of uniaxially oriented elasticizable fibers;
bonding at least some of the textile fibers to at least some of the elasticizable fibers to form a non-woven web; and heating the non-woven web to shrink and elasticize the elasticizable fibers whereby at least some of the textile fibers are gathered and pleated.
14. A non-woven web comprising:
a plurality of textile fibers; and a plurality of heat shrinkable elasticizable fibers with at least some of the elasticizable fibers being bonded to at least some of the textile fibers;
wherein said elasticizable fibers are adapted to shrink and gather and pleat the textile fibers upon application of heat to the web.
a plurality of textile fibers; and a plurality of heat shrinkable elasticizable fibers with at least some of the elasticizable fibers being bonded to at least some of the textile fibers;
wherein said elasticizable fibers are adapted to shrink and gather and pleat the textile fibers upon application of heat to the web.
15. The web according to claim 14, which further includes a plurality of melt blown fibers.
16. A fibrous elastomeric non-woven web comprising: a plurality of textile fibers having a modulus of elasticity of about 18 to 85 grams per denier which are gathered and pleated; and a plurality of heat shrunk elasticized fibers consisting essen-tially of an elasticized material with at least some of the elasticized fibers being bonded to at least some of the textile fibers.
17. The web according to claim 16, which further includes a plurality of melt blown fibers.
18. A fibrous non-woven web comprising:
a plurality of textile fibers having a modulus of elasticity of about 18 to 85 grams per denier; and a plurality of uniaxially oriented heat shrinkable elasticizable fibers consisting essentially of an elasticizable material with at least some of the elasticizable fibers being bonded to at least some of the textile fibers; and wherein said elasticizable heat shrinkable fibers are adapted to shrink to effect gathering and pleating of said textile fibers upon application of heat to the web.
a plurality of textile fibers having a modulus of elasticity of about 18 to 85 grams per denier; and a plurality of uniaxially oriented heat shrinkable elasticizable fibers consisting essentially of an elasticizable material with at least some of the elasticizable fibers being bonded to at least some of the textile fibers; and wherein said elasticizable heat shrinkable fibers are adapted to shrink to effect gathering and pleating of said textile fibers upon application of heat to the web.
19. The web according to claim 18, which further includes a plurality of melt blown fibers.
20. The web according to claim 16, comprising from about 5 percent to about 35 percent, by weight, of the elasticizable fibers and from about 65 percent to about 95 percent, by weight, of the textile fibers.
21. The web according to claim 16, wherein said elasticizable fibers are selected from the group consisting of styrene-butadiene copolymers, styren-butadiene-styrene copolymers and polyurethanes.
22. The web according to claim 16, wherein said textile fibers are selected from the group consisting of polyester fibers, polyamide fibers, glass fibers, polyolefin fibers, cellulosic derived fibers, acrylic polymer and copolymer fibers, natural-fibers and blends of two or more types of said textile fibers.
23. The web according to claim 22, wherein said polyamide fibers are selected from the group consisting of nylon fibers and acrylic polymer and copolymer fibers.
24. The web according to claim 22, wherein said polyolefin fibers are selected from the group consisting of polyethylene fibers and polypropylene fibers.
25. The web according to claim 22, wherein said cellulosic derived fibers are rayon fibers.
26. The web according to claim 22, wherein said natural fibers are selected from the group consisting of cotton fibers, wool fibers, pulp fibers, paper fibers and blends of two or more of said natural fibers.
27. The web according to claim 18, comprising from about 5 percent to about 35 percent, by weight, of the elasticizable fibers and from about 65 percent to about 95 percent, by weight, of the textile fibers.
28. The web according to claim 18, wherein said elasticizable fibers are selected from the group consisting of styrene-butadiene copolymers, styrene-butadiene-styrene copolymers and polyurethanes.
29. The web according to claim 18, wherein said textile fibers are selected from the group consisting of polyester fibers, polyamide fibers, glass fibers, polyolefin fibers, cellulosic derived fibers, acrylic polymer and copolymer fibers, natural fibers and blends of two or more types of said textile fibers.
30. The web according to claim 29, wherein said polyamide fibers are selected from the group consisting of nylon fibers.
31. The web according to claim 29, wherein said polyolefin fibers are selected from the group consisting of polyethylene fibers and polypropylene fibers.
32. The web according to claim 29, wherein said cellulosic derived fibers are rayon fibers.
33. The web according to claim 29, wherein said natural fibers are selected from the group consisting of cotton fibers, wool fibers, pulp fibers, paper fibers and blends of two or more of said natural fibers.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US69223185A | 1985-01-16 | 1985-01-16 | |
| US692,231 | 1985-01-16 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1298695C true CA1298695C (en) | 1992-04-14 |
Family
ID=24779757
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000499301A Expired - Lifetime CA1298695C (en) | 1985-01-16 | 1986-01-09 | Elasticized non-woven fabric and method of making the same |
Country Status (11)
| Country | Link |
|---|---|
| JP (1) | JPS61215754A (en) |
| KR (1) | KR920010333B1 (en) |
| CN (1) | CN86100754A (en) |
| AU (1) | AU584155B2 (en) |
| CA (1) | CA1298695C (en) |
| DE (1) | DE3601144A1 (en) |
| FR (1) | FR2576041B1 (en) |
| GB (1) | GB2169930B (en) |
| IT (1) | IT1190177B (en) |
| MX (1) | MX171146B (en) |
| SE (1) | SE8600157L (en) |
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|---|---|---|---|---|
| JPH0762302B2 (en) * | 1986-07-03 | 1995-07-05 | 株式会社クラレ | Fiber entangled body and its manufacturing method |
| JP2545260B2 (en) * | 1988-02-02 | 1996-10-16 | チッソ株式会社 | Bulky reinforced non-woven fabric |
| US4883549A (en) * | 1988-12-06 | 1989-11-28 | Kimberly-Clark Corporation | Method of attaching a composite elastic material to an article |
| JPH07122212B2 (en) * | 1988-12-13 | 1995-12-25 | ユニ・チャーム株式会社 | Bulky nonwoven fabric and method for producing the same |
| AU2772895A (en) * | 1994-07-26 | 1996-02-22 | Fiberweb North America, Inc. | Refastenable stretchable fastener system |
| US7047607B2 (en) | 1996-12-30 | 2006-05-23 | Wattex | Process for manufacturing a band-shaped non-woven product with increased tensile strength |
| BE1010827A3 (en) * | 1996-12-30 | 1999-02-02 | Wattex | Method for manufacturing of a non-woven with increased tensile and adjustable elasticity. |
| DE10212842A1 (en) * | 2002-03-11 | 2003-10-09 | Fibertex As Aalborg | Non-woven material with elastic properties |
| JP4918480B2 (en) * | 2004-04-23 | 2012-04-18 | インヴィスタ テクノロジーズ エスアエルエル | Elastic nonwoven sheet |
| CN102205677B (en) * | 2010-03-29 | 2014-05-28 | 厚生股份有限公司 | Process for forming fiber product with elasticity |
Family Cites Families (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB648644A (en) * | 1947-09-26 | 1951-01-10 | Us Rubber Co | Improvements in method of making elastic fabrics |
| NL227390A (en) * | 1957-04-30 | 1900-01-01 | ||
| FR1377289A (en) * | 1963-04-10 | 1964-11-06 | Method for milling multi-strand textile yarns of synthetic origin and method for treating fabrics made with such yarns | |
| GB1208785A (en) * | 1966-11-29 | 1970-10-14 | Monsanto Co | Non-woven fabric and method for preparation |
| US3651014A (en) * | 1969-07-18 | 1972-03-21 | Du Pont | Segmented thermoplastic copolyester elastomers |
| FR2134205B1 (en) * | 1971-04-26 | 1974-02-15 | Rhone Poulenc Textile | |
| US3766143A (en) * | 1971-06-21 | 1973-10-16 | Fmc Corp | Basic dyeable copolyester resins prepared from ortho and para isomersof lower alkyl sulfoalkoxy benzoates |
| US3763109A (en) * | 1971-08-19 | 1973-10-02 | Du Pont | Segmented thermoplastic copolyesters |
| NL180530C (en) * | 1974-01-30 | 1987-03-02 | Non Tisses Ste Fse | METHOD FOR MANUFACTURING A NON-WOVEN FABRIC AND FLAW OBTAINED BY THIS PROCESS |
| US4107364A (en) * | 1975-06-06 | 1978-08-15 | The Procter & Gamble Company | Random laid bonded continuous filament cloth |
| JPS58109613A (en) * | 1981-12-18 | 1983-06-30 | Teijin Ltd | Novel elastic fiber, its aggregate and production |
| CA1224608A (en) * | 1982-06-07 | 1987-07-28 | Biax Fiberfilm Corporation | Process and apparatus for forming non-woven webs from highly oriented melt blown fibers and products produced thereby |
| US4426420A (en) * | 1982-09-17 | 1984-01-17 | E. I. Du Pont De Nemours And Company | Spunlaced fabric containing elastic fibers |
| JPS59207182A (en) * | 1983-03-31 | 1984-11-24 | 日本バイリーン株式会社 | Production of extensible padding |
| EP0125494B1 (en) * | 1983-05-13 | 1992-01-02 | Kuraray Co., Ltd. | Entangled fibrous mat having good elasticity and production thereof |
| JPS59211666A (en) * | 1983-05-13 | 1984-11-30 | 株式会社クラレ | Interlaced nonwoven fabric good in extensibility and production thereof |
-
1986
- 1986-01-09 AU AU52118/86A patent/AU584155B2/en not_active Ceased
- 1986-01-09 CA CA000499301A patent/CA1298695C/en not_active Expired - Lifetime
- 1986-01-15 SE SE8600157A patent/SE8600157L/en unknown
- 1986-01-16 JP JP61007145A patent/JPS61215754A/en active Pending
- 1986-01-16 DE DE19863601144 patent/DE3601144A1/en not_active Ceased
- 1986-01-16 FR FR868600541A patent/FR2576041B1/en not_active Expired - Lifetime
- 1986-01-16 IT IT47541/86A patent/IT1190177B/en active
- 1986-01-16 CN CN198686100754A patent/CN86100754A/en active Pending
- 1986-01-16 GB GB8600951A patent/GB2169930B/en not_active Expired
- 1986-01-16 KR KR1019860000217A patent/KR920010333B1/en not_active IP Right Cessation
- 1986-01-23 MX MX001310A patent/MX171146B/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| GB2169930A (en) | 1986-07-23 |
| MX171146B (en) | 1993-10-05 |
| DE3601144A1 (en) | 1986-08-21 |
| AU5211886A (en) | 1986-07-24 |
| FR2576041B1 (en) | 1990-07-20 |
| JPS61215754A (en) | 1986-09-25 |
| GB2169930B (en) | 1989-06-07 |
| SE8600157D0 (en) | 1986-01-15 |
| KR920010333B1 (en) | 1992-11-27 |
| SE8600157L (en) | 1986-07-17 |
| GB8600951D0 (en) | 1986-02-19 |
| IT1190177B (en) | 1988-02-16 |
| KR860005916A (en) | 1986-08-16 |
| FR2576041A1 (en) | 1986-07-18 |
| IT8647541A0 (en) | 1986-01-16 |
| AU584155B2 (en) | 1989-05-18 |
| CN86100754A (en) | 1986-08-27 |
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