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EP0949371B1 - Etoffes non tissées de filaments et méthode de fabrication - Google Patents

Etoffes non tissées de filaments et méthode de fabrication Download PDF

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Publication number
EP0949371B1
EP0949371B1 EP99108935A EP99108935A EP0949371B1 EP 0949371 B1 EP0949371 B1 EP 0949371B1 EP 99108935 A EP99108935 A EP 99108935A EP 99108935 A EP99108935 A EP 99108935A EP 0949371 B1 EP0949371 B1 EP 0949371B1
Authority
EP
European Patent Office
Prior art keywords
filaments
nonwoven fabric
lactic acid
pressure
heat
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.)
Revoked
Application number
EP99108935A
Other languages
German (de)
English (en)
Other versions
EP0949371A2 (fr
EP0949371A3 (fr
Inventor
Koichi c/o Research and Development Center of UNITIKA LTD. Nagaoka
Fumio c/o Research and Development Center of UNITIKA LTD. Matsuoka
Naoji c/o Research and Development Center of UNITIKA LTD. Ichise
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Unitika Ltd
Original Assignee
Unitika Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=27478237&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0949371(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Priority claimed from JP25167995A external-priority patent/JP3434628B2/ja
Priority claimed from JP25608395A external-priority patent/JP3432340B2/ja
Priority claimed from JP25608095A external-priority patent/JP3710175B2/ja
Priority claimed from JP25607995A external-priority patent/JP3938950B2/ja
Priority to EP05022050.8A priority Critical patent/EP1612314B2/fr
Application filed by Unitika Ltd filed Critical Unitika Ltd
Publication of EP0949371A2 publication Critical patent/EP0949371A2/fr
Publication of EP0949371A3 publication Critical patent/EP0949371A3/fr
Publication of EP0949371B1 publication Critical patent/EP0949371B1/fr
Application granted granted Critical
Anticipated expiration legal-status Critical
Revoked legal-status Critical Current

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    • 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
    • D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/541—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres
    • D04H1/5412—Composite fibres, e.g. sheath-core, sea-island or side-by-side; Mixed fibres sheath-core
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
    • D04H3/147—Composite yarns or filaments
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30—Conjugate filaments; Spinnerette packs therefor
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • D01F6/625—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters derived from hydroxy-carboxylic acids, e.g. lactones
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • 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
    • D04H1/435—Polyesters
    • 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
    • D04H1/43825—Composite fibres
    • D04H1/43828—Composite fibres sheath-core
    • 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
    • D04H1/43912—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 fibres with noncircular cross-sections
    • 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
    • D04H1/43914—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 hollow fibres
    • 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
    • D04H1/44—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 the fleeces or layers being consolidated by mechanical means, e.g. by rolling
    • D04H1/46—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 the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
    • D04H1/48—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 the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres in combination with at least one other method of consolidation
    • 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
    • D04H1/54—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 by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/542—Adhesive fibres
    • D04H1/55—Polyesters
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005—Synthetic yarns or filaments
    • D04H3/009—Condensation or reaction polymers
    • D04H3/011—Polyesters
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/018—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the shape
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
    • D04H3/16—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic filaments produced in association with filament formation, e.g. immediately following extrusion

Definitions

  • the present invention relates generally to filament nonwoven fabrics which are degradable due to microorganisms and the like in natural environments and a method of manufacturing the same. More particularly, the invention relates to a degradable filament nonwoven fabric which can be produced from a biodegradable polymer composed principally of a thermoplastic aliphatic polyester under particular conditions, and a method of manufacturing the same.
  • nonwoven fabrics which are degradable due to microorganisms have been known including, for example, biodegradable nonwoven fabrics made from natural or regenerated filaments, such as cotton, flax, hemp, ramie, wool, rayon, chitin, and alginic acid filaments.
  • degradable nonwoven fabrics which are generally hydrophilic and water absorptive, are not suitable for use in such an application as disposable diaper top sheet, wherein- it is required that the fabric be hydrophobic and less water absorptive and should have a dry feel when it gets wet.
  • Another problem is that such nonwoven fabrics are very much liable to deterioration in strength and dimensional stability under wet environmental conditions; and this has limited the possibility, of exploiting new uses for such nonwoven fabrics in general industrial material applications. Further, such nonwoven fabrics, because of their non-thermoplastic nature, have no thermoformability and are therefore less processable.
  • microbially degradable filaments which may be obtainable by the melt spinning technique from a microbially degradable polymer having thermoplastic and hydrophobic characteristics, and microbially degradable nonwoven fabrics made up of such filaments.
  • a group of polymers generally called aliphatic polyesters are attracting high attention because they have microbial degradation characteristics.
  • such polymers include, for example, poly- ⁇ -hydroxyalkanoate as represented by microbially degradable polyester, poly- ⁇ -hydroxyalkanoate as represented by polycaprolactone, polyalkylene dicarboxylate composed of a polycondensate of glycol and dicarboxylic acid, such as polybutylene succinate, or copolymers of these polymers.
  • poly- ⁇ -hydroxyalkanoate as represented by microbially degradable polyester
  • poly- ⁇ -hydroxyalkanoate as represented by polycaprolactone
  • polyalkylene dicarboxylate composed of a polycondensate of glycol and dicarboxylic acid, such as polybutylene succinate
  • copolymers of these polymers include, for example, poly- ⁇ -hydroxyalkanoate as represented by microbially degradable polyester, poly- ⁇ -hydroxyalkanoate as represented by polycaprolactone, polyalkylene dicarboxylate composed of a polycondensate of glycol and dicarbox
  • polylactic acid in particular has a relatively high melting point such that, when a nonwoven fabric comprised of that material would prove to be very useful in applications which require heat resistance. As such, much expectation is now entertained for possibilities of polylactic nonwoven fabrics for practical use.
  • a polylactic nonwoven fabric is already disclosed in JP-A-7-126970 in which is described a staple filament nonwoven fabric composed principally of polylactic acid.
  • JP-A-6-212511 there is given a teaching about a polylactic staple filament material useful for the manufacture of polylactic staple filament nonwoven fabrics.
  • the manufacture of such a staple filament nonwoven fabric involves many operating stages, from melt spinning and up to nonwoven fabric forming; and this poses a problem from the standpoint of production cost economy.
  • JP-A-6-264343 which pertains to a biodegradable agricultural filament assembly, there is no detailed statement as to such important manufacturing conditions as filament drafting speed, and other necessary particulars, nor is there any teaching on the properties of the nonwoven fabric produced.
  • the teaching of International Nonwovens Journal, Vol. 7, No. 2, pp 69 (1995 ) is merely such that hard and brittle plate-like, polylactic spun bonded fabrics were obtained.
  • EP 0637641 (A1) there is no teaching that a polylactic spun bonded fabric having good flexibility and high mechanical strength can be produced.
  • the present invention is intended to solve the foregoing problems and has as its primary object the provision of a filament nonwoven fabric degradable due to microorganisms and the like in natural environments and yet having sufficient mechanical strength for practical use.
  • a nonwoven fabric made up of filaments comprised of a biodegradable polymer composed principally of a polylactic acid-based polymer or a polyalkylene dicarboxylate, wherein the filaments are partially bonded with heat and pressure or the filaments are three-dimensionally-entangled af ter partially bonded wi th heat and pressure and wherein the filaments have a crystallization degree of from 7 to 40 % and a supercool index of 0.4 or more.
  • a method of fabricating a nonwoven fabric made up of filaments comprised of a biodegradable polymer composed principally of a polylactic acid-based polymer or polyalkylene dicarboxylate which comprises the steps of melting the biodegradable polymer, said biodegradable polymer having a melt flow rate of 10 to 100 g/10 minutes as measured at 190°C according to ASTM-D-1238 (E), in a temperature range of from (Tm + 20)°C to (Tm + 80)°C, where Tm°C is the melting point of the biodegradable polymer; extruding the melt through a spinneret into filaments; drafting the extruded filaments by means of a suction device disposed below the spinneret under a quenching air blow generated through a conventional quenching device at a drafting speed of from 1,000 to 5,000 m/minute, thereby fining them down into finer filaments; then depositing such filaments, as they
  • the nonwoven fabric in accordance with the present invention is formed from filaments obtained through the process of rapid filament quenching beneath the spinneret and filament drafting at a drafting speed of from 1,000 to 5,000 m/minute, the filaments having a crystallization degree of from 7 to 40 % and a supercool index of 0.4 or more.
  • This ensures good flow behavior during the process of thermoforming, especially when the thermoforming operation involves complex and acute-angled shaping.
  • the nonwoven fabric exhibits less torsion stress and high breaking extension at thermoforming temperatures. This provides an advantage that any breakage which would otherwise possibly occur at times of thermoforming can be effectively prevented.
  • the nonwoven fabric has a three-dimensional entangled structure
  • various types of thermoformed products of such a filament nonwoven fabric have a larger specific surface area than thermoformed articles of known sheet materials and can be composted in a very short time.
  • this feature enables the filament nonwoven fabric of the invention to find its way into the markets for formed products of which air/liquid permeability is required, as well as those of which fibrous or nonwoven fabric-like hand is required.
  • Filaments employed in the present invention are preferably comprised of a polylactic acid-based polymer.
  • polylactic acid-based polymer a polymer having a melting point of 100°C or more selected from the group consisting of poly(D-lactic acid), poly(L-lactic acid), copolymers of D-lactic acid and L-lactic acid, copolymers of D-lactic acid and hydroxy-carboxylic acid, and copolymers of L-lactic acid and hydroxy-carboxylic acid, the selected polymer having a melting point of 100°C or more, or a blend of such polymers.
  • a plasticizer be added thereto especially for enhancement of spinnability during the process of spinning and flexibility improvement with respect to the resulting filaments and nonwoven fabric.
  • useful plasticizers for such purposes include triacetin, lactic acid oligomers, and dioctyl phthalate.
  • the amount of addition of such a plasticizer should be from 1 to 30 % by weight, preferably from 5 to 20 % by weight.
  • polylactic acid-based polymer is a copolymer of lactic acid and hydroxy-carboxylic acid
  • examples of hydroxy-carboxylic acid include glycolic acid, hydroxybutanoic acid, hydroxyvaleric acid, hydroxypentanoic acid, hydroxycaproic acid, hydroxyheptanoic acid, and hydroxyoctanoic acid.
  • hydroxycaproic acid or glycolic acid is particularly preferred from the standpoints of microbial degradation performance and cost economy.
  • polylactic acid-based polymers may be used alone or in the form of a blend of two or more kinds.
  • conditions such as polymers to be mixed and mixing proportions may be suitably determined in consideration of spinnability and other factors.
  • Such polymers each may be added with various additives, such as dulling agent, pigment, and crystallizing agent, as required within the limits in which the advantageous feature of the invention will not be affected.
  • each constituent filament of the nonwoven fabric may have any cross-sectional configuration, such as solid and otherwise. More specifically, it is preferable that the filament has one of such cross-sectional configurations as hollow section, odd-shaped section, sheath-core type composite section, and slit type composite section.
  • Fig. 1 shows a cross sectional view in which filament 1 has a hollow cross section.
  • Reference numeral 2 designates a filament portion
  • 3 designates a hollow portion.
  • the nonwoven fabric has good degradation capability. The reason is that as microorganisms and moisture erode inward from the outer circumferential portion for entry into the hollow portion 3 through holes formed in the filament portion 2 so that the surface area per unit polymer weight is so enlarged as to enhance the rate of degradation by microorganisms and the like.
  • a filament having an hollow section exhibits good performance for enhancement of quenching efficiency with respect to filaments spun, because per-unit-time polymer passage through a quenching region during spinning operation is relatively small in weight terms, and because the filament contains therein air bubbles of a small specific heat.
  • the filament has a polygonal odd-shaped cross section or a planar odd-shaped cross section as shown in Figs. 2 and 3
  • such sectional configuration can enhance filament quenching and spreading-open efficiency in the spinning stage, and can provide improved degradability with respect to the nonwoven fabric to be obtained.
  • the reason for this is that where a filament has an odd-shaped sectional configuration, the filament provides a larger surface area per unit polymer weight.
  • the filament cross section is a sheath-core type composite section
  • filaments of a sheath-core structure be formed of two kinds of components including the one filament component, the two kinds of components being arranged in such a manner that one having a higher melting point (hereinafter referred to as high melting point component) is used to assume a core position, the other of a lower melting point (hereinafter referred to as low melting point component) being used to assume a sheath position.
  • the melting point difference between the two components is determined in such a manner that for the core component, the melting point of one of the constituent polymers of the blend which has a lowermost melting point is taken as a basis, whereas for the sheath component, the melting point of one of the constituent polymers of the blend which has the highest melting point is taken as a basis.
  • the resulting nonwoven fabric can have good flexibility.
  • the filament cross section is a split type composite section
  • a nonwoven fabric formed from filaments of such a cross-sectional configuration can exhibit good degradability and good flexibility.
  • split type composite section refers to a filament section such that the filament comprises two kinds of filament components arranged in divisions separate from one another in a circumferential direction of the filament section, the two kinds of filament components including at least one of a polylactic acid-based polymer and a blend of plural kinds of polylactic acid-based polymers, chosen as one filament component, wherein both components extend continuously in the longitudinal direction of the filament and are exposed to the exterior of the filament.
  • cross-sectional configurations as shown in Figs. 4 to 6 may be exemplified. More particularly, Fig.
  • Fig. 4 shows a cross section wherein two components of filament 1, that is, high melting point component 4 and low melting point component 5 have respective radially extending divisions arranged in alternate relation.
  • Fig. 5 shows a cross section wherein low melting point component 5 constitutes a center portion of filament 1 and wherein high melting point component 4 has a plurality of divisions arranged along a circumferential edge of the low melting point component 5 in such a way that they protrude outward of the low melting point component 5.
  • a nonwoven fabric formed from filaments of such cross-sectional configuration will have improved degradability.
  • Fig. 5 shows a cross section wherein two components of filament 1, that is, high melting point component 4 and low melting point component 5 have respective radially extending divisions arranged in alternate relation.
  • Fig. 5 shows a cross section wherein low melting point component 5 constitutes a center portion of filament 1 and wherein high melting point component 4 has a plurality of divisions arranged along a circumferential edge of the low melting point component 5
  • a filament cross section which is similar to the one shown in Fig. 4 but is different in that there is provided an hollow portion 3.
  • Such filament configuration provides for further improvement in degradability, and filament quenching and spreading-open efficiency.
  • split type composite section it is possible as well to carry out fusion bonding in a temperature range near the melting point of low melting point component 5 during the process of web bonding with heat and pressure. In this operation, no fusion is caused to high melting point component 4. Thus, it is possible to obtain a nonwoven fabric having good flexibility.
  • various other odd-shaped composite cross-sectional configurations may be used including, for example, triangular, quadrangular, hexagonal, planar, Y-shaped, and T-shaped.
  • a web is partially bonded with heat and pressure without individual filaments being joined at intersection points, so that the web can retain a sheet-like configuration of nonwoven structure.
  • Such a nonwoven fabric has good flex properties because the constituent filaments are bonded only in partially formed fusion-bonded areas.
  • filaments are previously partially bonded with heat and pressure, whereby filaments are enabled to temporarily retain a web form for purposes of subsequent three-dimensionally entangling.
  • the nonwoven fabric obtained can have improved shape retention and improved dimensional stability.
  • filaments are separated entirely or at least partially by a subsequent entangling treatment, so that filaments including the separated filaments can make up a three-dimensional entanglement formation.
  • the fabric obtained possesses such mechanical strength and dimensional stability as can meet the requirements for practical use. Additionally, the fabric retains larger parts of non-fusion-bonded areas and can, therefore, also have good flexibility.
  • the nonwoven fabric of the invention can be efficiently manufactured by the so-called spun bond process.
  • a polylactic acid-based polymer of the above mentioned type having a melt flow rate of 10-100 g/10 minutes as measured at a temperature of 190°C in accordance with ASTM-D-1238 (E) is melted in a spinning temperature range of from (Tm + 20)°C to (Tm + 80)°C, where Tm°C is the melting point of the polymer, and the melt is spun into filaments through a spinneret which provides a desired filament cross section.
  • the filaments obtained are quenched by means of a conventional quenching device known in the art, such as horizontal blow type or annular blow type, and then the filaments are drafted by a suction device, such as air sucker, in an air stream of from 1,000 to 5,000 m/min. to the desired fineness.
  • a suction device such as air sucker
  • Masses of filaments discharged from the suction device are spread open each other and then deposited while being spread open each other on a travelling collector device, such as a screen conveyor, being thus formed into a web. Then, the web formed on the travelling collector device is subjected to heat treatment. A nonwoven fabric is thus obtained.
  • the polymer used should be melted within a temperature range of from (Tm + 20)°C to (Tm + 80)"C, where Tm°C is the melting point of the polymer.
  • Tm °C should be a melting point which is the highest of the melting points of the constituent polymers of the blend. If the spinning temperature is lower than (Tm + 20) °C, drafting operation in high-speed air currents will be of low efficiency.
  • the drafting speed be within the range of from 1,000 to 5,000 m/min.
  • the drafting speed may be suitably selected according to the MFR value of the polymer. If the drafting speed is less than 1,000 m/min., oriented crystallization of the polymer is retarded, which may result in inter-filament adhesion; and therefore the resulting nonwoven fabric is likely to have hard feel and inferior mechanical strength. If the drafting speed is more than 5,000 m/min., the process of drafting is forced to be carried out in excess of a critical drafting limit, and this results in filament break occurrences, it being thus difficult to maintain stable operation.
  • a partial bonding apparatus with heat and pressure is used to give partial bonding with heat and pressure at a temperature lower than the melting point which is the lowest of the melting points of polymeric components of the filament.
  • the expression "partially bonding with heat and pressure” means formation of fusion bonded areas by embossing or ultrasonic fusion bonding. Specifically, a web is passed through a clearance between a heated embossing roll and a flat surface metal roll for formation of inter-filament fusion bonded areas.
  • individual bonded areas with heat and pressure as particular partial areas in a web, each have an area of 0.2 to 15 mm 2 which may be of any configuration, such as circular, elliptic, diamond, triangular, T-shaped, and number sign-shaped.
  • the density of distribution of such areas that is, the density of bonded areas with heat and pressure is within the range of 4 to 100 bonded areas per cm 2 . If the density of bonded areas with heat and pressure is less than 4 bonded areas per cm 2 , no improvement can be had in the mechanical strength and shape retention capability of the resulting nonwoven fabric. If the density is more than 100 bonded areas per cm 2 , the resulting nonwoven fabric is rough and hard and has only poor flexibility.
  • the ratio of total bonded area with heat and pressure to total surface area of the web should be 3 to 50 %, though it depends upon the area of each individual pressure bonded area. If the pressure bonded area ratio is less than 3 %, the resulting nonwoven fabric cannot have improved mechanical strength or improved form retention capability. If the pressure bonded area ratio is more than 50 %, the resulting nonwoven fabric is rough and hard and has only poor flexibility.
  • Operating temperature for bonding with heat and pressure that is, the surface temperature of the embossing roll, as already stated, must be lower than the melting point of the polymer used.
  • the web to be bonded with heat and pressure is formed from filaments comprised of a blend of two or more kinds of polylactic acid-based polymers, or where the web is formed from bicomponent filaments having a composite cross-sectional configuration, for example, such a sheath-core type composite section or a split type composite section as earlier mentioned
  • the melting point of one polymer whose melting point is the lowest of those of all component polymers of the blend, or the melting point of one component of the bicomponent composite cross section which is lower than that of the other is taken as a reference, and operation must be carried out at an operating temperature lower than such a melting point.
  • the operating temperature exceeds that temperature limit, there may occur polymer adhesion to the bonding apparatus with heat and pressure, with the result that operating efficiency is adversely affected.
  • the resulting nonwoven fabric has a very hard hand, it being thus impractical to obtain a reasonably flexible nonwoven fabric.
  • the ultrasonic fusion bonding apparatus comprises an ultrasonic oscillator having a frequency of about 20 kHz which is generally called "horn", and a pattern roll having raised projections arranged circumferentially thereon in a area pattern or belt-like pattern.
  • the pattern roll is disposed below the ultrasonic oscillator so that partial hot fusion bonding can be effected by passing a web through a nip between the ultrasonic oscillator and the pattern roll.
  • Raised projections arranged on the pattern roll may be of a single row or plural rows. In the case of plural-row arrangement, the raised projections may be arranged either in parallel rows or in staggered rows. -
  • the manufacturing method is as described below.
  • a web formed on the travelling deposition apparatus in manner as earlier described is subjected to partial bonding with heat and pressure by a partial bonding apparatus with heat and pressure in an operating temperature range of from (Tm - 80)°C to (Tm - 50)°C, where (Tm)°C represents the melting point of one component polymer which is the lowest of the melting points of all component polymers of the filaments of the web, with linear pressure of a roll set within the range of from 10 to 100 kg/cm, whereby temporary bonded areas with heat and pressure are formed.
  • Aforesaid previously formed partial bonded areas with heat and pressure are preferably such that individual bonded areas with heat and pressure have an area of 0.2 to 15 mm 2 , with the density of fusion bonded areas therein being 4 - 100 bonded areas per cm 2 , preferably 5 - 80 bonded areas per cm 2 . If the density of fusion bonded areas is less than 4 bonded areas per cm 2 , any improvement cannot be obtained in mechanical strength and configurational retention property of the web after heat / pressure bonding. If the density exceeds 100 bonded areas per cm 2 , the processability of the web for three-dimensional entangling treatment is unsatisfactory.
  • the pressure bonded area ratio is 3-50 %, preferably 4-40 %.
  • the pressure bonded area ratio is less than 3 %, any improvement in dimensional stability cannot be obtained with respect to the resulting nonwoven fabric. Conversely, if the ratio is hither than 50 %, it is likely that the web is less processable for the purpose of three-dimensional entangling.
  • aforesaid conditions of operating temperature and a linear pressure of a roll set are particularly important. If the operating temperature is lower than (Tm - 80)°C and/or if the linear pressure of a roll set is lower than 5 kg/cm, the effect of bonding with heat and pressure is unsatisfactory, and no improvement can be achieved in respect of shape retention performance and dimensional stability of the resulting nonwoven fabric.
  • partial temporary bonded areas with heat and pressure serve to improve the shape retaining performance and mechanical strength of the web after bonding with heat and pressure and to facilitate process handling during three-dimensional entangling operation.
  • the partial temporary bonded areas with heat and pressure have a certain degree of bonding capability such that individual filaments at such areas can be easily separated at least partially by a mechanical external force applied during the three-dimensionally entangling operation.
  • the three-dimensional entangling treatment which is given after partial temporary bonding with heat and pressure is carried out through a treatment of pressured liquid stream in which the web is subjected to the action of pressure liquid streams, or through needle punching operation.
  • a web produced by the earlier mentioned spun bond process which is formed with partial temporary bonded areas with heat and pressure, is placed on a moving porous support plate and is exposed to the action of pressured liquid streams, whereby individual filaments, including at least partially separated filaments at bonded areas with heat and pressure, are three-dimensionally entangled so that all constituent filaments of the web are integrated as a whole.
  • an apparatus including an orifice having plural jet holes arranged in one row or plural rows, the jet holes having a bore diameter of from 0.05 to 2.0 mm, preferably from 0.1 to 0.4 mm, adjacent jet holes being 0.3-10 mm spaced apart, is employed. Jet streams of pressured liquid are delivered in a jet pressure range of from 5 to 150 kg/cm 2 G. If the pressure of liquid streams is less than 5 kg/cm 2 G, it is difficult to partially separate bonded areas with heat and pressure. Therefore, entangling of constituent filaments cannot be effected to any sufficient extent. If the pressure is higher than 150 kg/cm 2 G, individual filaments are too densely entangled, and the resulting nonwoven fabric is likely to be less flexible.
  • Jet holes should be arranged in a row along a direction orthogonal to the direction of advance of the web.
  • jet holes are arranged in plural rows, they are preferably arranged in staggered relation from the standpoint of subjecting the web to uniform action of pressured liquid streams.
  • Orifices having jet holes arranged therein may be arranged in plurality.
  • the distance between the jet holes and the web should be from 1 to 15 cm. If the distance is less than 1 cm, the texture of the resulting nonwoven fabric is rendered irregular. If the distance is more than 15 cm, the impact force of liquid streams, upon their impingement against the web, is so low that three-dimensional entangling is not sufficiently effected.
  • a support element for supporting the web during pressured liquid treating operation may be, for example, a wire cloth or mesh screen of 10 to 300 mesh, or a porous plate, but is not limited thereto, it being only required that the support element should permit pressured liquid streams to penetrate through the web.
  • the web subjected to entangling treatment on one side according to the above described method may be turned over and again subjected to entangling treatment by pressured liquid streams.
  • any known method may be used. For example, it is possible to mechanically remove any residual water to some degree by using a squeezing device, such as mangle roll, and then remove the rest of the water content by employing a dying apparatus, such as continuous hot air drier. Such drying operation may be carried out as ordinary dry heat treatment, but where required, may be carried out as wet heat treatment.
  • treating conditions such as drying temperature and drying time, in carrying out drying operation, conditions may be selected not only for the purpose of moisture removal, but also to allow reasonable degree of shrinkage with respect to the nonwoven web.
  • a web produced according to the spun bond process, with partial temporary bonded areas with heat and pressure formed thereon, is punched through by punch needles so that filaments including at least partially separated filaments at those areas bonded with heat and pressure are three-dimensionally entangled for integration as a whole.
  • Needle punching is preferably carried out under the conditions of; needle depth, 5-50 mm; punching density, 50-400 punches/cm 2 . If the needle depth is less than 5 mm, the degree of entanglement of filaments is insufficient, which in turn results in poor dimensional stability, while a needle depth of more than 50 mm poses a problem from the standpoint of productivity. If the punch density is less than 50 punches/cm 2 , constituent filaments at bonded areas with heat and pressure may not be smoothly separated and entangling of filaments may not sufficiently be effected; and the resulting nonwoven fabric may lack dimensional stability.
  • punch density is more than 400 punches / cm 2 , filament breaks due to punch needles may occur and the resulting nonwoven fabric may be of lower mechanical strength.
  • Punch needles are selectable in respect of thickness, length, number of barbs, barb pattern. etc. according to the single filament fineness, intended use, etc.
  • Aforesaid pressured liquid stream treatment is applicable to products of lower weight per unit area (15 - 200 g/m 2 ), and by such treatment it is possible to obtain nonwoven fabrics having good flexibility and high mechanical strength.
  • Needle punch treatment is applicable to products of higher weight per unit area (100 - 500 g/m 2 ), and by such treatment it is possible to obtain having good flexibility, good air permeability, and good water permeability.
  • the reason for selection of applicable treatment according to the weight per unit area is that there is some difference in web penetration capability between pressured liquid streams and needle punches.
  • the pressured bonded area density is 20 bonded areas per cm 2 or less, preferably 10 bonded areas per cm 2 or less, and the pressure bonded area ratio is 15 % or less, preferably 10 % or less.
  • a filament nonwoven fabric having such fusion bonded areas can take advantage of the presence of non-fusion-bonded areas to effectively provide filament to filament entangling through the three-dimensionally entangling treatment.
  • the nonwoven fabric can exhibit good dimensional stability and high mechanical strength. In case that fusion bonded areas partially remain in existence, such fusion bonded areas adds to the dimensional stability and mechanical strength of the nonwoven fabric.
  • a nonwoven fabric of the invention is comprised of filaments spun from a biodegradable polymer composed principally of a thermoplastic aliphatic polyester, the filaments having a crystallization degree of from 7 to 40 % and a supercool index of 0.4 or more.
  • a method of fabricating a nonwoven fabric made up of filaments comprised of a biodegradable polymer composed principally of a thermoplastic aliphatic polyester comprises the steps of melting the biodegradable polymer, said biodegradable polymer having a melt flow rate of from 10 to 100 g/10 minutes as measured at 190°C according to ASTM-D-1238 (E), in a temperature range of from (Tm + 20)°C to (Tm + 80)°C, where Tm°C is the melting point of the biodegradable polymer; extruding the melt through a spinneret into filaments; drafting the extruded filaments by means of a suction device disposed below the spinneret under a quenching air blow generated through a conventional quenching device and at a drafting speed of from 1,000 to 5,000 m/minute, thereby fining them down into finer filaments: then depositing such filaments, as they are spread open each other, and are laid up on a travelling collector
  • filaments used in the invention are formed from a biodegradable polymer composed principally of a thermoplastic aliphatic polyester.
  • thermoplastic aliphatic polyesters include poly( ⁇ -hydroxy acid), such as polyglycolic acid or polylactic acid, ahd copolymers of repeating units mentioned above or constituents of such polymers.
  • polycondensates of glycol and dicarboxylic acid may be mentioned as such, including, for example, polyethylene oxalate, polyethylene succinate, polyethylene adipate, polyethylene azelate, polybutylene oxalate, polybutylene succinate, polybutylene adipate, polybuylene sebacate, polyhexamethylene sebacate, polyneopentyl oxalate, and polyalkylene dicarboxylate copolymer comprising any of these as repeating units.
  • polylactic acid-based polymer any one of polybutylene succinate, polyethylene succinate, polybutylene adipate, and polybutylene sebacate, or copolymers in which these polymers are included as repeating units are preferred from the standpoints of biodegradability, spinnability or the like.
  • the aliphatic polyester is a polylactic acid-based polymer, specifically, any one of poly(D-lactic acid), poly(L-lactic acid), copolymer of D-lactic acid and L-lactic acid, copolymer of D-lactic acid and hydroxycarboxylic acid, and copolymer of L-lactic acid and hydroxycarboxylic acid which has a melting point of 100°C or more is preferred.
  • the hydroxy-carboxylic acid may be, for example, glycolic acid, hydroxybutyric acid, hydroxyvaleric acid, hydroxypentanoic acid, hydroxycaproic acid, hydroxyheptanoic acid, or hydroxyoctanoic acid.
  • the number-average molecular weight of the polylactic acid-based polymer is preferably 50,000 - 95,000.
  • aliphatic polyester is polyalkylene dicarboxylate
  • any polymer selected from the group consisting of polybutylene succinate, polyethylene succinate, polybutylene adipate, and polybutylene sebacate, or a copolymer in which such polymers are included as repeating units is preferred as such.
  • a copolymer of not less than 70 mol % of butylene succinate and one of ethylene succinate, butylene adipate, and butylene sebacate is preferred.
  • Such biodegradable polymers as above enumerated may be used in a blend of plural selected polymers.
  • thermoplastic aliphatic polyester and aliphatic polyamide such as polycapramide (nylon 6), polytetramethylene adipamide (nylon 46), polyhexamethylene adipamide (nylon 66), polyundecanamide (nylon 11), and polylauramide (nylon 12), that is, an aliphatic polyester amide-based copolymer.
  • biodegradable polymer should have a number-average molecular weight of not less than about 20,000, preferably not less than 40,000, more preferably not less than 60,000.
  • Polymers which are chain-extended with a small amount of diisocyanate or tetracarboxylic dianhydride to enhance polymerization degree may also be used.
  • the biodegradable polymer may be added with various kinds of additives, such as dulling agent, pigment, and crystallizing agent, as required, but within the limits which are not detrimental to the intended effects.
  • additives such as dulling agent, pigment, and crystallizing agent
  • crystallizing agents such as talc, boron nitride, calcium carbonate, magnesium carbonate, and titanium oxide is desirable, because it can prevent inter-filament blocking at spinning and quenching stages, and because it can enhance crystallization during thermoforming operation and improve heat resistance and mechanical strength characteristics
  • the amount of such addition is within the range of from 0.1 to 3.0 wt %, more preferably from 0.5 - 2.0 wt %.
  • the filament configuration of constituent filaments of the nonwoven fabric may be solely of aliphatic polyester or may be of a composite of two or more kinds of alphatic polyesters.
  • the filament cross section of constituent filaments may be a usual circular section, an irregular section, an hollow section, or a composite section such as sheath-core type section, as stated above.
  • the single filament fineness of constituent filaments of the nonwoven fabric is preferably 20 denier or less, more preferably 1 to 12 denier. If the fineness is more than 20 denier, filament quenching at the spinning stage is hindered, and in addition the flexibility characteristics of the resulting nonwoven fabric are unfavorably affected. This is inconvenient from the standpoint of thermoforming operation with the nonwoven fabric, because the fabric does not allow smooth working especially when some complex and acute-angled deformation work is involved.
  • the weight per unit area of the nonwoven fabric is preferably within the range of 10 to 500 g/m 2 . If the weight per unit area is less than 10 g/m 2 , the nonwoven fabric is of poor appearance and insufficient in mechanical strength, being unsatisfactory for practical use. If the weight per unit area is more than 500 g/m 2 , flexibility is affected. Where finer single filament is involved, the fabric is of greater denseness than a nonwoven fabric of the same weight per unit area which is made up of filaments of coarser single filament. However, the fact that deterioration in mechanical strength due to biodegradation is faster must be taken into consideration. Where the mechanical strength of the filament itself is low, a larger weight per unit area is required in order to enable the fabric to maintain a certain degree of strength.
  • Constituent filaments of the nonwoven fabric of the invention should have a crystallization range of from 7 to 40 % and a supercool index of 0.4 or more. This is basic requirements for affording efficient working during thermoforming operation, especially at the time of complex and acute angle deformation work.
  • a crystallization degree is determined from a wide-angle X-ray diffraction pattern of powdered filament according to the Ruland method. Whilst, a supercool index is expressed by an equation based on a fusion enareaherm curve (heat up/melting and heat down), details of which will be described hereinafter. These are reference indices as to formability. Where a crystallization degree is less than 7 %, fusion breakage is likely to occur at a high deformation region. If a crystallization degree is more than 40 %, heat deformation is less likely to occur, which makes it difficult to carry out high drafting forming. Where a supercool index is less than 0.4, the nonwoven fabric lacks transformation ability during thermoforming operation.
  • constituent filaments of the nonwoven fabric means that the nonwoven fabric is acceptable for thermoforming operation with it. This in turn means that strain-stress is low at the thermoforming temperature and elongation at break is high. Therefore, the nonwoven fabric can be prevented from breaking during thermoforming operation.
  • elongation at break of the nonwoven fabric is 20 % or more, preferably 30 % or more, more preferably, 40 % or more.
  • the filament nonwoven fabric and constituent filaments thereof are not liable to shrink during thermoforming operation.
  • the reason is that if any shrinking of the web sheet occurs at the time of forming, the sheet is taken up by the mold, which prevents stable continuos forming operation. Therefore, the shrinked area of the nonwoven fabric at the time of thermoforming operation is not more than 10%, preferably not more than 5 %, more preferably not more than 2 %.
  • the nonwoven fabric of the invention maintains a sheet-form configuration having a nonwoven structure because of the fact that the web is subjected to heat treatment.
  • One configurational feature of the nonwoven fabric of the invention is that the web is partially bonded with heat and pressure.
  • the nonwoven fabric of such configuration in accordance of the invention has good flexibility performance, because the fabric is bonded only at the fusion bonded areas. This provides for maintenance of smooth working capability during thermoforming operation, especially at the time of complex and accute-angled deformation work, and also provides for improvement in the form retention capability of the nonwoven-fabric during thermoforming operation.
  • Another configurational feature of the nonwoven fabric of the invention is such that the fabric has fusion bonded areas formed when individual filaments at preformed partial temporary bonded areas with heat and pressure were partially separated through three-dimensional entangling treatment, and such that individual filaments at non-fusion-bonded portions in areas other than the fusion bonded areas are three-dimensionally entangled so that the fabric is integrated as a whole.
  • a still another configurational feature of the nonwoven fabric of the invention is such that individual filaments at preformed partial temporary bonded areas with heat and pressure are completely separated and three-dimensionally entangled through three-dimensional entangling treatment and are integrated as a whole.
  • a biodegradable polymer must have an MFR value measured according to the method stated in ASTM-D-1238 (E) which is within the range of 10 - 100 g/10 min. If the MFR value is less than 10 g/10 min., the melt viscosity is too high and therefore the efficiency of drafting by air sucker or the like is poor, which may be a cause of filament break at the spinning stage. If the MFR value is more than 100 g/10 min., the melt viscosity is too low, which leads to poor drafting efficiency, it being thus difficult to carry out operation in stable condition.
  • Spinning temperature should be suitably selected by taking into consideration the type of polymer, MFR value of the polymer, or the like. If the spinning temperature is too low, the result is poor drafting efficiency. If the spinning temperature is too high, interfilament adhesion may be caused, resulting in poor filament-spreading-out effect; and in addition, thermal decomposition of the polymer itself will proceed.
  • the suction device is preferably set at a location below and at 1 to 2 m distance from the spinneret. Where necessary, earlier mentioned crystallizing agent may be added to enhance quenching effect.
  • the drafting speed be within the range of 1,000 to 5,000 m / min. Through such arrangement, it is possible to achieve a crystallization degree of from 7 to 40 % with respect to constituent filaments of the nonwoven fabric and a supercool index of 0.4 or more. If the drafting speed is less than 1,000 m/min., crystallization of oriented polymers will not progress so that the crystallization degree of filaments may be less than 7 %, thus resulting in lower mechanical strength of the resulting nonwoven fabric.
  • the drafting speed is more than 5,000 m/min.
  • crystallization of oriented polymers will progress excessively so that the crystallization degree of filaments may exceed 40 % and, in addition, the supercool index may be lower than 0.4.
  • the filaments are subject to higher strain-stress at thermal deformation temperatures, which leads to poor thermoformability. Therefore, it is especially preferable that the drafting speed be 1,200 to 3,000 m/min.
  • the operating temperature for bonding with heat and pressure that is, the surface temperature of the embossing roll is preferably lower than the melting point of one polymer having lowest melting point in case that the web is comprised of plural kinds of polymers. If the operating temperature exceeds this temperature, polymer adhesion to the bonding apparatus with heat and pressure may occur, which adversely affects operating efficiency. Moreover, the resulting nonwoven fabric feels hard and is less adaptable to a mold having a complex configuration, leading to poor formability.
  • pressure bonded area ratio for bonding with heat and pressure may be from 3 to 50 %. If this ratio is less than 3 %, the resulting fabric will have poor form retention property necessary for fabric handling purposes and poor dimensional stability. If.this ratio is more than 50 %, the resulting nonwoven fabric feels hard and is less adaptable to a mold having a complex configuration, leading to poor formability.
  • This partial bonding with heat and pressure may be carried out in a continuous process operation or in a separate operation stage.
  • the choice of either method may be determined suitably, for example, according to the formed product to be manufactured using the nonwoven fabric obtained.
  • Another method for heat treatment of webs is such that temporary bonded areas with heat and pressure are formed by applying a partial bonding treatment with heat and pressure to the web; then individual filaments at the temporary bonded areas with heat and pressure are partially separated by effecting three-dimensional entangling treatment ; then individual filaments in separated state are three-dimensionally entangled into overall integration.
  • a partial bonding operation with heat and pressure for forming temporary bonded areas with heat and pressure is carried out by pressing the web by means of the embossing roll.
  • it is important that such bonding operation is carried out at an operating temperature of from (Tm - 80)°C to (Tm - 50)°C, where Tm°C is the melting point of the polymer having the lowest melting point of the component polymers, with the linear pressure of a roll set at 10 - 100 kg/cm.
  • thermoforming operation using the biodegradable filament nonwoven fabric as a material.
  • the component polymer of the nonwoven fabric, or the nonwoven fabric are comprised of plural polymers, one polymer having the highest melting point of the polymers is taken as a subject polymer, and the nonwoven fabric is preheated at a temperature higher than the glass transition temperature of, but lower than the melting point of the subject polymer, being then subjected to pressed forming in a mold. Thereafter, for improving the mechanical strength of the resulting formed piece, crystallization is enhanced at temperatures in the vicinity of the crystallizing temperature.
  • MFR Melt Flow Rate
  • Weight per unit area (g/m 2 ) From each sample in standard condition were prepared 10 specimens, each of 10 cm x 10 cm. After the moisture content of each specimen was brought to equilibrium, each specimen was weighed for determining the weight (g) thereof. The average of the values obtained was converted into a value per unit area, which was defined as weight per unit area (g/m 2 ).
  • Filament crystallization degree (%) Measured according to a wide-angle X-ray diffraction method (powdered; Ruland Method).
  • the wide-angle X-ray diffraction method diffracted X-ray interference intensity measurements were made in the direction of reflection angle 2 ⁇ , whereby an diffracted intensity curve was obtained. Then, from the diffracted intensity curve were separated to a crystal-based diffracted peak and an amorphous portion-based dispersion halo, which were quantitatively determined.
  • Air permeability (cc / cm 2 /sec.): Measured according to the Frazir type method described in JIS-L-1096. More specifically, 3 specimens, each of 15 cm in length and 15 cm in width, were prepared. A Frazir type tester was used in such a way that, after a specimen was attached to one end of a cylinder, a suction pump adjustment was made by means of a variable resistor so as to allow an inclined type barometer to give a pressure reading of 12.7 mmH 2 O. Then, the quantity of air passing through the specimen (cc/cm 2 /sec.) was determined on the basis of pressure readings of a vertical type barometer and according to the type of air spouting orifice used. Average value with respect to three specimens was taken as air permeability.
  • a polybutylene succinate (number-average molecular weight: 50,000) having a melting point of 116°C and an MFR value of 30 g/10 min., and containing 1 wt % of talc, was used.
  • This polymer was melt spun through a circular spinneret at a spinning temperature of 190°C and at a mass out flow rate from each orifice of 0.67 g/min. Filaments spun were quenched by a conventional quenching device, and were then drafted and attenuated at a drafting speed of 2,000 m/min. Filaments were spread open each other and deposited on a collecting surface of a travelling conveyor, being thus formed into a web.
  • the web was then passed through a partial bonding apparatus with heat and pressure comprising embossing rolls wherein partial bonding with heat and pressure was carried out under the following conditions: roll temperature of 90°C; and pressure bonded area ratio of 7.6 %.
  • roll temperature of 90°C The constituent filaments of the web had a crystallization degree of 18 % and a supercool index of 0.41.
  • the filament nonwoven fabric obtained was preheated to 80°C and by using a mold the preheated nonwoven fabric was formed into a conical coffee filter having an opening diameter of 8.5 cm and a depth of 4.5 cm.
  • This coffee filter was a good formed piece.
  • the formed piece had an air permeability of 120 cc/cm 2 /sec.
  • the formed filter was put into a continuous composting arrangement, and in about one month it had been composted leaving no trace of it.
  • This polymer was melt spun through a spinneret identical to the one used in Example 1 at a spinning temperature of 200°C and at a mass out flow rate from each orifice of 0.89 g/min. Filaments spun were quenched by a conventional quenching device, and were then drafted and attenuated at a drafting speed of 2,000 m/min.
  • Filaments were spread open each other and deposited on a travelling conveyor, being thus formed into a web.
  • the web was then passed through a partial bonding apparatus with heat and pressure comprising embossing rolls wherein partial bonding with heat and pressure was carried out under the conditions of roll temperature, 132°C, and pressure bonded area ratio, 6.5 %.
  • a filament nonwoven fabric comprised of filaments having a single filament fineness of 4.0 denier, with a weight per unit area of 65 g/m 2 , was obtained.
  • the constituent filaments of the web had a crystallization degree of 21 % and a supercool index of 0.52.
  • the filament nonwoven fabric obtained was preheated to 120°C and was formed by pressing into a plant pot having an opening diameter of 10.5 cm and a depth of 5.5 cm. In this way, good formed piece was obtained.
  • the formed plant pot had an air permeability of 170 cc/cm 2 /sec.
  • a plant potted in this formed plant pot was set, together with the pot, for growth in the ground at an intended location. The plant smoothly grew into a mature tree. Three years after the plant in the plant pot was initially set in the ground, it was found that the plant pot had been degraded in the earth with no trace left of it.
  • the two components were melt spun through a spinneret having a nozzle configuration such that in a split type composite cross section as shown in Fig. 5 , the low melting point component was disposed at the core side and the high melting point component at the leaf side, with a spinning temperature set at 170°C and a mass out flow rate from each orifice of 1.36 g/min. Filaments spun were quenched by a conventional quenching device, and were then drafted and attenuated at a drafting speed of 1,500 m/min., then spread open each other and deposited on a collecting surface of a travelling conveyor.
  • the filaments were subjected to temporary bonding with heat and pressure under the conditions of: embossing temperature, 51°C; linear pressure of a roll set, 10 kg/cm; pressure bonded area ratio, 6.5 %; and pressure bonded spot density, 36 bonded areas per cm 2 , whereby a nonwoven web was formed.
  • the web was subjected to a three-dimensionally-entangling treatment by pressured liquid streams. That is, the nonwoven web was placed on a moving wire net (of 48 mesh) and exposed to jet streams of pressure liquid.
  • an apparatus having orifices arranged in three rows, each orifice having a hole diameter of 0.2 mm and inter-hole spacing of 0.4 mm, was employed.
  • Example 3 For the pressure liquid, water was used. Two kinds of jet pressure were used, namely, 40 kg / cm 2 G ⁇ 4 times (Example 3), and 100 kg / cm 2 G ⁇ 4 times (Example 4). Excess water in the web was removed by means of mangle rolls, and then the web was dried.
  • Example 3 in which the jet pressure applied was 40kg/cm 2 G, the nonwoven fabric obtained was a three-dimensionally entangled nonwoven fabric, with temporary bonded areas with heat and pressure left unremoved.
  • Example 4 in which the jet pressure applied was 100 kg / cm 2 G, the nonwoven fabric obtained had constituent filaments thereof three-dimensionally entangled all over, with temporary bonded areas with heat and pressure completely separated. These nonwoven fabrics had a weight per unit area of 70. g/m 2 . Their constituents filaments had a single-filament fineness of 3.5 denier, a crystallization degree of 16 %, and a supercool index of 0.6.
  • the filament nonwoven fabrics thus obtained were each preheated to 100°C and formed by pressing into a plant pot having an opening diameter of 10.5 cm and a depth of 5.5 cm. In this way, good formed pieces were obtained.
  • the formed plant pots, of both Examples 3 and 4 had an air permeability of about 160 cc/cm 2 sec.
  • a plant potted in each formed plant pot was set, together with the pot, for growth in the ground at an intended location. The plant smoothly grew into a mature tree. Three years after the plant in the plant pot was initially set in the ground, it was found that the plant pot had been degraded in the earth with no trace left of it.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Nonwoven Fabrics (AREA)

Claims (19)

  1. Etoffe non tissée consistant en filaments constitués d'un polymère biodégradable composé principalement d'un polymère à base d'acide polylactique ou d'un polyalkylène dicarboxylate, où les filaments sont partiellement liés grâce à la chaleur et à la pression ou bien les filaments sont entremêlés dans les trois dimensions après avoir été partiellement liés grâce à la chaleur et la pression et où les filaments présentent un degré de cristallisation de 7 à 40 % et un indice de super-refroidissement de 0,4 ou plus.
  2. Etoffe non tissée selon la revendication 1, dans laquelle le polymère biodégradable comprend un polymère sélectionné parmi le groupe constitué de poly(acide D-lactique), de poly(acide L-lactique), de copolymères d'acide D-lactique et d'acide L-lactique, de copolymères d'acide D-lactique et d'acide hydroxycarboxylique, et de copolymères d'acide L-lactique et d'acide hydroxycarboxylique, ou d'un mélange de tels polymères.
  3. Etoffe non tissée selon la revendication 1, dans laquelle le polymère biodégradable est un polymère sélectionné parmi le groupe constitué de polysuccinate de butylène, de polysuccinate d'éthylène, de polyadipate d'éthylène, et de polysébacate de butylène, ou d'un copolymère dans lequel de tels polymères sont présents en tant que principales unités qui se répètent.
  4. Etoffe non tissée sont la revendication 1, dans laquelle le polymère biodégradable se voit ajouter un agent de cristallisation.
  5. Etoffe non tissée selon la revendication 1, dans laquelle l'étoffe non tissée comporte des zones liées par fusion par points de sorte que les filaments individuels au niveau des zones liées temporairement préformées partiellement grâce à la chaleur et à la pression sont partiellement séparés les uns des autres par un traitement d'entremêlement dans les trois dimensions et dans laquelle les filaments individuels au niveau de zones autres que les zones liés par fusion de manière par points, qui ne sont pas liées par fusion, sont entremêlés dans les trois dimensions ensemble de manière à être intégrés en un tout.
  6. Etoffe non tissée selon la revendication 1, dans laquelle les filaments individuels au niveau de zones temporairement liées préformées partiellement grâce à la chaleur et la pression sont complètement séparés les uns des autres par un traitement d'entremêlement dans les trois dimensions, grâce à quoi ils sont entrelacés dans les trois dimensions les uns les autres de manière à être intégrés en un tout.
  7. Etoffe non tissée selon la revendication 1, dans laquelle l'étoffe non tissée est thermoformable.
  8. Etoffe non tissée selon la revendication 7, dans laquelle le polymère biodégradable comprend un polymère sélectionné parmi le groupe constitué de poly(acide D-lactique), de poly(acide L-lactique), de copolymères d'acide D-lactique et d'acide L-lactique, de copolymères d'acide D-lactique et d'acide hydroxycarboxylique, et de copolymères d'acide L-lactique et d'acide hydroxycarboxylique ou un mélange de tels polymères, ledit polymère à base d'acide polylactique ayant un nombre de masse moléculaire moyen de 50 000 à 95 000.
  9. Procédé de fabrication d'une étoffe non tissée consistant en filaments constitués d'un polymère biodégradable composé principalement d'un polymère à base d'acide polylactique ou d'un polyalkylène dicarboxylate, comprenant les étapes consistant à faire fondre le polymère biodégradable, ledit polymère biodégradable ayant une vitesse d'écoulement à l'état fondu de 10 à 100 g/10 min telle que mesurée à 190°C conformément à la norme ASTM-D-1238 (E) dans une plage de températures de (Tm + 20)°C à (Tm + 80)°C, où Tm°C est le point de fusion du polymère biodégradable, à extruder le bain de fusion au travers d'une filière en filaments, à étirer les filaments extrudés au moyen d'un dispositif d'aspiration disposé au-dessous de la filière sous un souffle d'air de trempe généré par le biais d'un dispositif classique et à une vitesse d'étirage de 1 000 à 5 000 m/min, en les affinant ainsi en filaments plus fins, à déposer ensuite les mêmes filaments, tels qu'ils sont étalés ouverts les uns aux autres, et sont disposés sur une surface de dispositif de recueil qui se déplace pour former un tissu, et à effectuer un traitement par la chaleur du tissu afin d'obtenir ainsi l'étoffe non tissée.
  10. Procédé de fabrication selon la revendication 9, dans lequel le polymère biodégradable est un polymère sélectionné parmi le groupe constitué de poly(acide D-lactique), de poly(acide L-lactique), de copolymères d'acide D-lactique et d'acide L-lactique, de copolymères d'acide D-lactique et d'acide hydroxycarboxylique, et de copolymères d'acide L-lactique et d'acide hydroxycarboxylique, ou d'un mélange de tels polymères.
  11. Procédé de fabrication selon la revendication 9, dans lequel le polymère biodégradable est un polymère sélectionné parmi le groupe constitué du polysuccinate de méthylène, du polysuccinate d'éthylène, du polyadipate de butylène, et du polysébacate de butylène, ou d'un copolymère dans lequel de tels polymères sont présents en tant que principales unités qui se répètent.
  12. Procédé de fabrication selon la revendication 9, dans lequel un agent de cristallisation est ajouté au polymère biodégradable.
  13. Procédé de fabrication selon la revendication 9, dans lequel les filaments constitutifs du tissu sont partiellement liés grâce à la chaleur et à la pression à une température inférieure au point de fusion du polymère biodégradable.
  14. Procédé de fabrication selon la revendication 13, dans lequel deux ou plus types de composants constitués dudit polymère biodégradable sont filés par fusion en filaments au moyen d'une filière qui procure une configuration en coupe composite en ce qui concerne la section transversale de chacun des filaments, et dans lequel ladite liaison partielle grâce à la chaleur et à la pression est effectuée à une température inférieure au point de fusion de l'un desdits deux ou plus types de composants qui est le plus bas de leurs points de fusion.
  15. Procédé de fabrication selon la revendication 9, qui comprend en outre lé fait de soumettre le tissu à une liaison partielle grâce à la chaleur et à la pression afin de former ainsi des zones temporairement liées grâce à la chaleur et à la pression, en effectuant ensuite un traitement d'entremêlement dans les trois dimensions par rapport au tissu afin d'amener ainsi les filaments individuels au niveau des zones temporairement liées grâce à la chaleur et à la pression à être au moins partiellement séparés, et les filaments individuels entremêlés dans les trois dimensions dans la condition séparée afin d'intégrer ainsi des filaments du tissu comme un tout.
  16. Procédé de fabrication selon la revendication 15, dans lequel l'étape de liaison partielle grâce à la chaleur et à la pression pour former des zones temporairement liées grâce à la chaleur et à la pression est exécutée en pressant le tissu par le biais d'un rouleau de gaufrage, ladite liaison partielle grâce à la chaleur et à la pression étant effectuée à une température de traitement de (Tm - 80)°C à (Tm - 50)°C, où Tm°C est le point de fusion de l'un des composants des filaments constitutifs qui est le plus bas des points de fusion des composants, la pression linéaire de l'ensemble de rouleaux se trouvant dans une plage de 10 à 100 kg/cm.
  17. Procédé de fabrication selon la revendication 9, dans lequel l'étoffe non tissée obtenue est soumise à un traitement de thermoformage.
  18. Procédé de fabrication selon la revendication 9, dans lequel le polymère biodégradable comprend un polymère à base d'acide polylactique, ledit polymère à base d'acide polylactique étant un polymère sélectionné parmi le groupe constitué de poly(acide D-lactique), de poly(acide L-lactique), de copolymères d'acide D-lactique et d'acide L-lactique, de copolymères d'acide D-lactique et d'acide hydroxycarboxylique, et de copolymères d'acide L-lactique et d'acide hydroxycarboxylique, ou d'un mélange de tels polymères, ledit polymère à base d'acide polylactique ayant un nombre de masse moléculaire moyen de 50 000 à 95 000.
  19. Procédé de fabrication selon la revendication 9, dans lequel la vitesse d'étirage du fait du dispositif d'aspiration au cours du traitement d'étirage est de 1 200 à 3 000 m/min.
EP99108935A 1995-09-29 1996-09-16 Etoffes non tissées de filaments et méthode de fabrication Revoked EP0949371B1 (fr)

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JP25167995A JP3434628B2 (ja) 1995-09-29 1995-09-29 ポリ乳酸系長繊維不織布およびその製造方法
JP25167995 1995-09-29
JP25608095A JP3710175B2 (ja) 1995-10-03 1995-10-03 ポリ乳酸系長繊維不織布およびその製造方法
JP25607995 1995-10-03
JP25608395 1995-10-03
JP25607995A JP3938950B2 (ja) 1995-10-03 1995-10-03 ポリ乳酸系長繊維不織布およびその製造方法
JP25608095 1995-10-03
JP25608395A JP3432340B2 (ja) 1995-10-03 1995-10-03 生分解性成形用長繊維不織布およびその製造方法
EP96114791A EP0765959B1 (fr) 1995-09-29 1996-09-16 Etoffes non-tissée de filaments et sa méthode de fabrication

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Publication number Publication date
EP0765959B1 (fr) 2000-01-19
EP1612314A2 (fr) 2006-01-04
EP1612314B2 (fr) 2014-01-08
EP0949371A2 (fr) 1999-10-13
EP1612314A3 (fr) 2006-11-22
EP0765959A1 (fr) 1997-04-02
KR970021415A (ko) 1997-05-28
EP0949371A3 (fr) 2004-05-12
KR100406244B1 (ko) 2004-03-30
EP1612314B1 (fr) 2009-09-09

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