US20050056956A1 - Process for forming micro-fiber cellulosic nonwoven webs from a cellulose solution by melt blown technology and the products made thereby - Google Patents

Process for forming micro-fiber cellulosic nonwoven webs from a cellulose solution by melt blown technology and the products made thereby Download PDF

Info

Publication number
US20050056956A1
US20050056956A1 US10/663,117 US66311703A US2005056956A1 US 20050056956 A1 US20050056956 A1 US 20050056956A1 US 66311703 A US66311703 A US 66311703A US 2005056956 A1 US2005056956 A1 US 2005056956A1
Authority
US
United States
Prior art keywords
solvent
solution
bath
hydro
jets
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.)
Abandoned
Application number
US10/663,117
Inventor
Rongguo Zhao
Eckhard Schwarz
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.)
Biax Fiberfilm Corp
Original Assignee
Biax Fiberfilm Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Biax Fiberfilm Corp filed Critical Biax Fiberfilm Corp
Priority to US10/663,117 priority Critical patent/US20050056956A1/en
Publication of US20050056956A1 publication Critical patent/US20050056956A1/en
Assigned to BIAX FIBERFILM CORPORATION reassignment BIAX FIBERFILM CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ZHAO, RONGGUO
Abandoned legal-status Critical Current

Links

Images

Classifications

    • 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
    • D01D5/12—Stretch-spinning methods
    • D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
    • 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
    • D01D4/00—Spinnerette packs; Cleaning thereof
    • D01D4/02—Spinnerettes
    • D01D4/025—Melt-blowing or solution-blowing dies
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D—TEXTILES; PAPER
    • 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
    • D04H18/00—Needling machines
    • D04H18/04—Needling machines with water jets

Definitions

  • This invention relates to a process of melt blowing a cellulose solution through a concentric melt blown die with a plurality of spinning nozzles to form cellulosic microfiber webs with different web structures.
  • Lyocell fibers are man-made fibers regenerated from a proper cellulose solution (dope) with different techniques.
  • Lyocell fiber is one of the regenerated, man-made cellulose fibers. It is traditionally made by a dry-jet-wet-spinning process, where the cellulose solution of a solvent, such as N-methyl morpholine N-oxide, is extruded through a spinneret to form filaments. These filaments travel a short distance in air (the dry-jet), then get into a coagulation bath for regeneration. A proper mechanical pulling force is applied onto the regenerated fibers to attenuate the fiber in the “dry-jet” section.
  • a solvent such as N-methyl morpholine N-oxide
  • Regenerated fibers then go through a series of washing/finishing baths and drying units to form final products in the form of continuous filaments or short fibers.
  • Jurkovic et al., in U.S. Pat. No 5,252,284 and Michels et al., in U.S. Pat. No. 5,417,909 deal especially with the geometry of extrusion nozzles for spinning cellulose dissolved in NMMO.
  • Brandner et al., in U.S. Pat. No. 4,426,228, is exemplary of a considerable number of patents that disclose the use of various compounds to act as stabilizers in order to prevent cellulose and/or solvent degradation.
  • U.S. Pat. No. 6,306,334 teaches a process using much larger sectioned spinning orifices compared with the above referenced technologies enabling a higher dope throughput per orifice to minimize tendency for orifice plugging problem.
  • Example of this patent described a single orifice melt blown die with air delivered from both sides of the die through parallel slots at an angle of 30 degree, it failed to teach more details of a die with multiple orifices, such as that how the orifices are arranged, and how the air applied to extruded filaments. Due to the unique characteristic of cellulose-NMMO solution and complexity of MB technology, it is uncertain that if the same results from a single orifice MB die could be obtained from a multiple orifice MB die.
  • the present invention is directed to a process of melt blowing a cellulose solution through a concentric melt blown die with multiple rows of spinning nozzles to form cellulosic microfiber webs with different web structures.
  • cellulose as used here should be understood as either cellulose from natural resources or a synthetic polymer blend with cellulose.
  • die is often used as the term of “spinneret” in this invention.
  • concentric melt blown die refers to an apparatus described in U.S. Pat. No 5,476,616 with the hot air nozzles concentric with the polymer spinning nozzles and the air flows parallel with the polymer filaments near the exits of the nozzles.
  • the cellulose solution is extruded out through each spinning nozzle at a proper temperature (ranging from 80 to 140° C.) and a proper throughput.
  • the extrudates are attenuated quickly by high velocity hot air jets from a few hundred micrometers in diameter to a few micrometers in diameter within a few centimeters from the nozzle exits.
  • These microfibers are collected on the surface of a moving collecting device, which can be either a drum collector or a flat screen collector.
  • a set of jets of solvent/non-solvent mixture shoots from a series of fine orifices/nozzles on the flying fibers and the collected web.
  • solvent used in the present invention refers to NMMO, dilute caustic soda, phosphoric acid, mixture of liquid ammonia/ammonia thiocynate and others.
  • non-solvent used here refers to water, alcohol (C n H 2n+1 OH, n ⁇ 10), and/or water/alcohol/solvent solutions.
  • water is often used as the term of “non solvent” in this invention.
  • the jets of solvent/non-solvent solution serves two functions in this process, coagulating (fully or partially) the filaments and hydro-entangling the filaments to form webs.
  • the final cellulose microfibers have an average fiber diameter ranging from 1 micrometer to 20 micrometer with a relatively broad fiber diameter distribution
  • Spinning nozzles have an inside diameter in the range of 0.005-0.050 inch with a length/diameter (L/D) ratio in the range of 40-300. Under proper operation conditions, the resultant melt blown web is free of “shot”, a defect in the form of glob of polymer which is significantly large than the fiber. Fibers produced by the method of this invention possess desirable crimps.
  • FIG. 1 is a schematic view of a melt blowing spinneret with multiple rows of spinning nozzles and concentric air jets used with the invention.
  • FIG. 2 is a schematic bottom view of part of the melt blowing spinneret in FIG. 1 .
  • FIG. 3 is a diagram of the equipment used with the above melt blowing spinneret.
  • FIGS. 4, 5 and 6 are optical micrographs of melt blown Lyocell nonwoven at 40 ⁇ , 100 ⁇ and 400 ⁇ , respectively.
  • the process of the present invention is suitable to various cellulose solutions.
  • the solvent includes NMMO, dilute caustic soda, phosphoric acid, mixture of liquid ammonia/ammonia thiocynate and others.
  • the ways making a solution of the cellulose are known to the art, as reported by Petrovan, Collier, and Negulescu in “Rheology of Cellulosic N-Methymorpholine Oxide Monohydrate Solutions of Different Degrees of Polymerization” (Journal of Applied Polymer Science, Vol 79, 396-405 (2001)), by Albrecht in “Lyocell Fibers” (Chemical Fiber International, Vol 47, 298-304 (1997)), by Luo in U.S. Pat.
  • FIG. 1 it shows a schematic view of a melt blowing spinneret.
  • the cellulose solution is supplied by an extruder and/or metering pump through the cavity 2 of the distribution plate 1 to the nozzle plate 4 .
  • the plate 4 includes a gas cavity 9 , which is supplied with hot compressed air or other fluids from 3 .
  • the baffle plates 8 divert the gas stream and force the gas through the gas distribution plate 5 and the air holes 13 of the top plate 7 . Plates 5 and 7 are separated with a spacer 6 .
  • the hot air jets 11 reach a sonic velocity at the air hole exit, even at supersonic levels depending on the spinneret geometry and the processing conditions.
  • the high velocity gas accelerates and attenuates the exiting cellulose NMMO solution 12 from the nozzles 10 to form fine fibers 12 a .
  • the nozzles made of high quality stainless steel, have a length ranging from 0.5′′ to 3′′, and inside diameter (I.D.) ranging from 0.005′′ to 0.050′′, and preferably, a length from 1′′ to 2′′ and an I.D ranging from 0.009′′ to 0.020′′.
  • the spacing of the nozzles is between 0.045′′ to 1.0′′, and preferably, between 0.050′′ to 0.2′′.
  • the length of the nozzle sticking out of the top plate is between ⁇ 0.005′′ to 1′′, and preferably, between 0.050′′ to 0.220′′.
  • FIG. 2 shows a portion of the spinneret bottom view.
  • the present process produces significantly more filaments per inch spinneret compared to the process disclosed in U.S. Pat. No. 6,306,334 B1 and U.S. Pat. No. 6,358,461 B1, where a melt blowing die of single row of spinning holes employed.
  • FIG. 3 shows an example of detailed melt blowing process of this invention.
  • the multiple row filaments of the cellulose solution are attenuated from a few hundred micrometers in diameter to a few micrometers in diameter within a short distance from the spinneret.
  • these molten microfibers 12 a are blown onto a paternally perforated moving surface 14 , which is located 3 inch to 50 inch from the spinneret.
  • two sets of jet heads 15 shoot high pressure/speed hydro jets 16 onto the fiber/air stream with an angle 17 to coagulate/regenerate and entangle the cellulose microfibers.
  • At least another set of jet heads 19 shooting hydro jets 20 is used down stream to enhance the integrity and properties of nonwoven web.
  • the term of “hydro jet” in the present invention refers to jets of pressured liquid or mixture of liquid/air.
  • these hydro-jets 16 and 20 are supplied with circulating solvent/non-solvent solution 26 from the first regenerating bath 27 by a high-pressure pump 44 .
  • the solvent/non-solvent solution applied to the nonwoven web will return to the first generating bath with the help of the gutter 42 .
  • the hydro-entangled web 22 guided by a roller 21 enters into the nip of pressure roller 23 and driving roller 24 travels in the first bath 27 for major regeneration.
  • the web 22 folds in layers on slow-moving conveyer screen 28 submerged in bath 27 .
  • the conveyer screens 28 and 28 a are supported by rollers 29 and 29 a .
  • the layered web 25 is submerged in solution 26 for at least 30 seconds, then enters into the nip of pressure roller 31 and driving roller 32 for liquid removing.
  • the squeezed web folds to form web layers 33 onto the conveyer screen 28 a in the bath 34 for further regeneration in fresh water. After at least 25 seconds, the web comes out of the bath 34 , gets washed with fresh water sprays 35 , and goes through the nip of 21 a and pressure roller 36 .
  • the washed and squeezed web travels with the collector surface 14 through a zone heated with heater 37 and vacuumed with a vacuum duct 38 and vacuum head 39 .
  • the dried Lyocell fiber nonwoven web is winded up as roll 41 on the surface of the collector.
  • At least one gutter 40 is attached to the vacuum duct to guide the penetrated solution back to the nonwoven web.
  • the solution in bath 27 and bath 34 is stirred constantly by helical stirrers 43 .
  • the optical micrographs shown in FIGS. 4-6 are of Lyocell fibers made by the process of the present invention.
  • the average fiber diameter is about 5 ⁇ 15 micrometers.
  • a 3 ⁇ 4 inch extruder is fed with a NMMO solution comprising 10.5% by weight cellulose, 77.5% by weight of NMMO and the rest is mainly water.
  • the solid solution are in the form of pellet of 0.05′′ ⁇ 0.08′′ in size.
  • the feeding hoper is filled with Argon gas to prevent moisture takeup.
  • the cellulose has an average degree of polymerization from 330 ⁇ 360.
  • the extruder has three heating zones and the temperatures were set as 165° F. (Zone 1 , near the feeding hoper), 210° F., 230° F., respectively.
  • the solution temperature and pressure at the spinneret were kept in 230° F. and 600 PSI, respectively.
  • the air temperature and pressure in the spinneret were held at 250° F. and 15 PSI respectively.
  • the solution throughput was about 0.16 gram/nozzle/min.
  • the attenuated microfibers are deposited on a perforated rotating drum right after contacted with the hydro needling jets. These strong needling jets serve as a pre-coagulation means and a fiber entangling means.
  • the web goes through another set of hydro needling jets for better mechanical bonding and regenerating. The well bonded web is regenerated, washed, post-treated, and air dried.
  • a 1 inch extruder is fed with a NMMO solution comprising 14% by weight cellulose, 76% by weight of NMMO and the rest is mainly water.
  • the solid solution are in the form of pellet of 0.05′′ ⁇ 0.08′′ in size.
  • the feeding hoper is filled with Argon gas to prevent moisture takeup.
  • the cellulose has an average degree of polymerization of 670.
  • the extruder has three heating zones and the temperatures were set as 185° F. (Zone 1 , near the feeding hoper), 230° F., 250° F., respectively.
  • the solution temperature and pressure at the spinneret were kept in 250° F. and 860 PSI, respectively.
  • the air temperature and pressure in the spinneret were held at 270° F. and 10 PSI respectively.
  • the solution throughput was about 0.8 gram/nozzle/min.

Abstract

This invention relates to a process of melt blowing a cellulose solution through a concentric melt blown die with multiple rows of spinning nozzles to form cellulosic microfiber webs with different web structures. The process comprises the steps of (a) extruding a cellulose solution (dope) through a melt blown spinneret with multiple rows of spinning nozzles; (b) drawing each individual extrudate filament to fine fiber diameter by its own air jet; (c) coagulating and entangling the fine fibers with a series of pressured hydro needling jets of recycling solution of the mixture of cellulose solvent and non-solvent in the spin-line; (d) collecting the stream of microfibers, air and needling jets on a moving collecting surface to form cellulosic fiber web; (e) hydro-entangling the said pre-bonded web downstream with at least one set of hydro needling jets of recycling solvent/non-solvent solution for forming well bonded nonwoven web; (f) regenerating the fine fibers in at least one bath for at least 5 seconds; (g) further regenerating and washing the fine fibers in another bath for at least 5 seconds; (h) pinching the well bonded melt blown cellulosic nonwoven with pressure rollers to remove major portions of the non-solvent; (i) drying the nonwoven web by heat, or vacuum or both, and (j) winding the nonwoven web into rolls.

Description

    CROSS-REFERENCE TO RELATED APPLICATIONS
  • (Not applicable)
    • STATEMENT REGARDING FEDERARALLY SPONSORED RESEARCH OR DEVELOPMENT
  • (Not Applicable)
    • REFERENCE TO SEQUENCE LISTING, A TABLE, OR A COMPUTER PROGRAM LISTING COMPACT DISC APPENDIX
  • (Not applicable)
    • BACKGROUND OF THE INVENTION
  • 1. Field of the Invention
  • This invention relates to a process of melt blowing a cellulose solution through a concentric melt blown die with a plurality of spinning nozzles to form cellulosic microfiber webs with different web structures.
  • 2. Description of the Prior Art
  • Cellulosic fibers are man-made fibers regenerated from a proper cellulose solution (dope) with different techniques. As an example, Lyocell fiber is one of the regenerated, man-made cellulose fibers. It is traditionally made by a dry-jet-wet-spinning process, where the cellulose solution of a solvent, such as N-methyl morpholine N-oxide, is extruded through a spinneret to form filaments. These filaments travel a short distance in air (the dry-jet), then get into a coagulation bath for regeneration. A proper mechanical pulling force is applied onto the regenerated fibers to attenuate the fiber in the “dry-jet” section. Regenerated fibers then go through a series of washing/finishing baths and drying units to form final products in the form of continuous filaments or short fibers. U.S. Pat. Nos. 4,142,913; 4,144,080; 4,211,574; 4,246,221, and 4,416,698 and others described the details of this process.
  • Jurkovic et al., in U.S. Pat. No 5,252,284 and Michels et al., in U.S. Pat. No. 5,417,909 deal especially with the geometry of extrusion nozzles for spinning cellulose dissolved in NMMO. Brandner et al., in U.S. Pat. No. 4,426,228, is exemplary of a considerable number of patents that disclose the use of various compounds to act as stabilizers in order to prevent cellulose and/or solvent degradation.
  • Zikeli et al., in U.S. Pat. Nos. 5,589,125 and 5,607,639, direct a stream of air transversely across strands of extruded lyocell dope as they leave the spinnerets. This air stream serves only to cool and does not act to stretch the filaments. French laid open application 2,735,794 describes formation of lyocell fibers by a process of melt blowing. However, these are highly fragmented microfibers useful principally for production of self bonded non-woven webs.
  • U.S. Pat. No. 6,306,334 teaches a process using much larger sectioned spinning orifices compared with the above referenced technologies enabling a higher dope throughput per orifice to minimize tendency for orifice plugging problem. Although Example of this patent described a single orifice melt blown die with air delivered from both sides of the die through parallel slots at an angle of 30 degree, it failed to teach more details of a die with multiple orifices, such as that how the orifices are arranged, and how the air applied to extruded filaments. Due to the unique characteristic of cellulose-NMMO solution and complexity of MB technology, it is uncertain that if the same results from a single orifice MB die could be obtained from a multiple orifice MB die.
    • SUMMARY OF THE INVENTION
  • The present invention is directed to a process of melt blowing a cellulose solution through a concentric melt blown die with multiple rows of spinning nozzles to form cellulosic microfiber webs with different web structures. The term of “cellulose” as used here should be understood as either cellulose from natural resources or a synthetic polymer blend with cellulose. The term of “die” is often used as the term of “spinneret” in this invention. The term of “concentric melt blown die” refers to an apparatus described in U.S. Pat. No 5,476,616 with the hot air nozzles concentric with the polymer spinning nozzles and the air flows parallel with the polymer filaments near the exits of the nozzles.
  • The cellulose solution is extruded out through each spinning nozzle at a proper temperature (ranging from 80 to 140° C.) and a proper throughput. The extrudates are attenuated quickly by high velocity hot air jets from a few hundred micrometers in diameter to a few micrometers in diameter within a few centimeters from the nozzle exits. These microfibers are collected on the surface of a moving collecting device, which can be either a drum collector or a flat screen collector. A set of jets of solvent/non-solvent mixture shoots from a series of fine orifices/nozzles on the flying fibers and the collected web. The term of solvent used in the present invention refers to NMMO, dilute caustic soda, phosphoric acid, mixture of liquid ammonia/ammonia thiocynate and others. The term of “non-solvent” used here refers to water, alcohol (CnH2n+1OH, n≦10), and/or water/alcohol/solvent solutions. The term “water” is often used as the term of “non solvent” in this invention. Depending on the position and angle of the non-solvent jet, the amount of non-solvent applied, and other factors, the resultant cellulose microfiber nonwoven web exhibits different characteristics. The jets of solvent/non-solvent solution serves two functions in this process, coagulating (fully or partially) the filaments and hydro-entangling the filaments to form webs.
  • The final cellulose microfibers have an average fiber diameter ranging from 1 micrometer to 20 micrometer with a relatively broad fiber diameter distribution
  • Spinning nozzles have an inside diameter in the range of 0.005-0.050 inch with a length/diameter (L/D) ratio in the range of 40-300. Under proper operation conditions, the resultant melt blown web is free of “shot”, a defect in the form of glob of polymer which is significantly large than the fiber. Fibers produced by the method of this invention possess desirable crimps.
  • There is an object of the present invention to provide a method of forming cellulose microfiber nonwoven fabrics from a solution of a cellulose solvent, such as NMMO, by utilizing melt blown technology with concentric multiple-row spinning nozzles
  • It is an additional object to provide a method for making the said nonwoven web without additional processes, i.e. carding, web forming, and bonding.
  • It is a further object to provide a method for making cellulose nonwovens with different web structures.
  • It is another object to provide a method for forming a biodegradable nonwoven web.
    • BRIEF DESCRIPTION OF THE DRAWINGS
  • The foregoing aspects and many of the attendant advantages of this invention will become more readily appreciated as the same becomes better understood by reference to the following detailed description, when taken in conjunction with the accompanying drawings, wherein:
  • FIG. 1 is a schematic view of a melt blowing spinneret with multiple rows of spinning nozzles and concentric air jets used with the invention.
  • FIG. 2 is a schematic bottom view of part of the melt blowing spinneret in FIG. 1.
  • FIG. 3 is a diagram of the equipment used with the above melt blowing spinneret.
  • FIGS. 4, 5 and 6 are optical micrographs of melt blown Lyocell nonwoven at 40×, 100× and 400×, respectively.
    • DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
  • The process of the present invention is suitable to various cellulose solutions. The solvent includes NMMO, dilute caustic soda, phosphoric acid, mixture of liquid ammonia/ammonia thiocynate and others. The ways making a solution of the cellulose are known to the art, as reported by Petrovan, Collier, and Negulescu in “Rheology of Cellulosic N-Methymorpholine Oxide Monohydrate Solutions of Different Degrees of Polymerization” (Journal of Applied Polymer Science, Vol 79, 396-405 (2001)), by Albrecht in “Lyocell Fibers” (Chemical Fiber International, Vol 47, 298-304 (1997)), by Luo in U.S. Pat. No 6,306,334 B1, and by Liu, Cuculo, Smith in “Diffusion competition between solvent and nonsolvent during the coagulation process of cellulose/ammonia/ammonium thiocynate fiber spinning system” (Journal of Polymer Science Part B: Polymer Physics Vol 28, Issue 4, Pages 449-465 (1990))
  • Reference to FIG. 1, it shows a schematic view of a melt blowing spinneret. The cellulose solution is supplied by an extruder and/or metering pump through the cavity 2 of the distribution plate 1 to the nozzle plate 4. The plate 4 includes a gas cavity 9, which is supplied with hot compressed air or other fluids from 3. The baffle plates 8 divert the gas stream and force the gas through the gas distribution plate 5 and the air holes 13 of the top plate 7. Plates 5 and 7 are separated with a spacer 6. The hot air jets 11 reach a sonic velocity at the air hole exit, even at supersonic levels depending on the spinneret geometry and the processing conditions. The high velocity gas accelerates and attenuates the exiting cellulose NMMO solution 12 from the nozzles 10 to form fine fibers 12 a. The nozzles, made of high quality stainless steel, have a length ranging from 0.5″ to 3″, and inside diameter (I.D.) ranging from 0.005″ to 0.050″, and preferably, a length from 1″ to 2″ and an I.D ranging from 0.009″ to 0.020″. The spacing of the nozzles is between 0.045″ to 1.0″, and preferably, between 0.050″ to 0.2″. The length of the nozzle sticking out of the top plate is between −0.005″ to 1″, and preferably, between 0.050″ to 0.220″. FIG. 2 shows a portion of the spinneret bottom view.
  • The present process produces significantly more filaments per inch spinneret compared to the process disclosed in U.S. Pat. No. 6,306,334 B1 and U.S. Pat. No. 6,358,461 B1, where a melt blowing die of single row of spinning holes employed.
  • FIG. 3 shows an example of detailed melt blowing process of this invention. The multiple row filaments of the cellulose solution are attenuated from a few hundred micrometers in diameter to a few micrometers in diameter within a short distance from the spinneret. With the high velocity air jets 11, these molten microfibers 12 a are blown onto a paternally perforated moving surface 14, which is located 3 inch to 50 inch from the spinneret. At a point in the spinline, two sets of jet heads 15 shoot high pressure/speed hydro jets 16 onto the fiber/air stream with an angle 17 to coagulate/regenerate and entangle the cellulose microfibers. At least another set of jet heads 19 shooting hydro jets 20 is used down stream to enhance the integrity and properties of nonwoven web. The term of “hydro jet” in the present invention refers to jets of pressured liquid or mixture of liquid/air. Through a set of cartridge filters 43 and transfer lines 18, these hydro- jets 16 and 20 are supplied with circulating solvent/non-solvent solution 26 from the first regenerating bath 27 by a high-pressure pump 44. The solvent/non-solvent solution applied to the nonwoven web will return to the first generating bath with the help of the gutter 42. The hydro-entangled web 22 guided by a roller 21 enters into the nip of pressure roller 23 and driving roller 24 travels in the first bath 27 for major regeneration. The web 22 folds in layers on slow-moving conveyer screen 28 submerged in bath 27. The conveyer screens 28 and 28 a are supported by rollers 29 and 29 a. The layered web 25 is submerged in solution 26 for at least 30 seconds, then enters into the nip of pressure roller 31 and driving roller 32 for liquid removing. The squeezed web folds to form web layers 33 onto the conveyer screen 28 a in the bath 34 for further regeneration in fresh water. After at least 25 seconds, the web comes out of the bath 34, gets washed with fresh water sprays 35, and goes through the nip of 21 a and pressure roller 36. The washed and squeezed web travels with the collector surface 14 through a zone heated with heater 37 and vacuumed with a vacuum duct 38 and vacuum head 39. The dried Lyocell fiber nonwoven web is winded up as roll 41 on the surface of the collector. At least one gutter 40 is attached to the vacuum duct to guide the penetrated solution back to the nonwoven web. The solution in bath 27 and bath 34 is stirred constantly by helical stirrers 43.
  • The optical micrographs shown in FIGS. 4-6 are of Lyocell fibers made by the process of the present invention. The average fiber diameter is about 5˜15 micrometers.
    • EXAMPLE 1
  • A ¾ inch extruder is fed with a NMMO solution comprising 10.5% by weight cellulose, 77.5% by weight of NMMO and the rest is mainly water. The solid solution are in the form of pellet of 0.05″˜0.08″ in size. The feeding hoper is filled with Argon gas to prevent moisture takeup. The cellulose has an average degree of polymerization from 330˜360.
  • The extruder has three heating zones and the temperatures were set as 165° F. (Zone 1, near the feeding hoper), 210° F., 230° F., respectively. The molten solution was forced into the body of a 5-inch-2-row spinneret, with 126 spinning nozzles (I.D.=0.009″) and protruding length of 0.1915″. The solution temperature and pressure at the spinneret were kept in 230° F. and 600 PSI, respectively. The air temperature and pressure in the spinneret were held at 250° F. and 15 PSI respectively. The solution throughput was about 0.16 gram/nozzle/min.
  • The attenuated microfibers are deposited on a perforated rotating drum right after contacted with the hydro needling jets. These strong needling jets serve as a pre-coagulation means and a fiber entangling means. The web goes through another set of hydro needling jets for better mechanical bonding and regenerating. The well bonded web is regenerated, washed, post-treated, and air dried.
    • EXAMPLE 2
  • A 1 inch extruder is fed with a NMMO solution comprising 14% by weight cellulose, 76% by weight of NMMO and the rest is mainly water. The solid solution are in the form of pellet of 0.05″˜0.08″ in size. The feeding hoper is filled with Argon gas to prevent moisture takeup. The cellulose has an average degree of polymerization of 670.
  • The extruder has three heating zones and the temperatures were set as 185° F. (Zone 1, near the feeding hoper), 230° F., 250° F., respectively. The molten solution was forced into the body of a 5-inch-2-row spinneret, with 63 spinning nozzles (I.D.=0.020″) and protruding length of 0.180″. The solution temperature and pressure at the spinneret were kept in 250° F. and 860 PSI, respectively. The air temperature and pressure in the spinneret were held at 270° F. and 10 PSI respectively. The solution throughput was about 0.8 gram/nozzle/min.
  • The inventors have herein described the best present mode of practicing their invention. It will be evident to others skilled in the art that many variations that have not been exemplified should be included within the broad

Claims (12)

1. A process for forming bonded cellulosic microfibers nonwovens comprises the steps of
(a) extruding a cellulose solution (dope) through a concentric melt blown spinneret with a plurality of spinning nozzles,
(b) drawing each individual extrudate filament to fine fiber diameter by its own air jet,
(c) coagulating and entangling the fine fibers with a series of pressured hydro needling jets of recycling solution of the mixture of cellulose solvent and non-solvent in the spin-line,
(d) collecting the stream of microfibers, air and needling jets on a moving collecting surface to form cellulosic fiber web,
(e) hydro-entangling the said pre-bonded web downstream with at least one set of hydro needling jets of recycling solvent/non-solvent solution for forming well bonded nonwoven web,
(f) regenerating the fine fibers in at least one bath for at least 5 seconds,
(g) further regenerating and washing the fine fibers in another bath for at least 5 seconds,
(h) pinching the well bonded melt blown cellulosic nonwoven with pressure rollers to remove major portions of the non-solvent.
(i) drying the nonwoven web by heat, or vacuum or both, and
(j) winding the nonwoven web into rolls.
2. The process of claim 1 in which the spinning nozzles are arranged in at least one row with a nozzle-to-nozzle space of 0.050″ to 1.000″
3. The process of claim 1 in which the spinning nozzles are 0.005″ to 0.050″ in inside diameter and 0.500″ to 3.000″ in length.
4. The process of claim 1 in which the spinning nozzles are concentric with their individual gas holes and protruded −0.005″ to 0.800″ from the top plate of the said gas holes.
5. The process of claim 1 in which the solvent of the cellulose solution is one or more of the following: NMMO, dilute caustic soda, phosphoric acid, mixture of liquid ammonia/ammonia thiocynate and others.
6. The process of claim 1 in which the non-solvent of cellulose is one or more of the following: water, alcohol (CnH2n+1OH, n≦10), and/or water/alcohol/solvent solutions
7. The process of claim 1 in which the recycling solvent/non-solvent solution is filtered and supplied from the regenerating bath by a high pressure pump and part of the solution is continuously removed from the said bath for solvent recycling.
8. The process of claim 1 in which the recycling NMMO solution is supplied to the needling jets from and come back to the first regenerating bath. The second washing bath is continuously filled with fresh non-solvent, which is sprayed onto the nonwoven web first. Part of the low concentration solution continuously overflow from the washing bath to the regenerating bath.
9. The collecting system for manufacturing the said cellulose fiber nonwoven comprises
(a) a paternally perforated drum with a diameter ranged from 20 inch to 70 inch
(b) at least one set of coagulating hydro needling jets, which contacts with flying fibers 0.5 inch to 30 inch from the collecting surface and at an angle from 5 degree to 75 degree (relative to the air blowing direction)
(c) at least another set of hydro needling jets downstream for both hydro-entangling and fiber regenerating.
(d) at least one regenerating bath and one washing bath with conveying belts.
(e) at least one vacuum section across and beneath the drum surface
(f) at least one heating section across and above the drum surface
10. The collecting system of claim 4 in which the regenerating and washing bathes contain series of rollers to guide the nonwoven web.
11. The conveying belt of claim 9 submerged in both bathes moves slower than surface speed of the collecting drum.
12. The cellulosic nonwovens of claim 1 in which the fibers are essentially continuous with an average size of 1 to 30 micrometer in diameter and bonded by both self-bonding and hydro-entanglement.
US10/663,117 2003-09-16 2003-09-16 Process for forming micro-fiber cellulosic nonwoven webs from a cellulose solution by melt blown technology and the products made thereby Abandoned US20050056956A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US10/663,117 US20050056956A1 (en) 2003-09-16 2003-09-16 Process for forming micro-fiber cellulosic nonwoven webs from a cellulose solution by melt blown technology and the products made thereby

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US10/663,117 US20050056956A1 (en) 2003-09-16 2003-09-16 Process for forming micro-fiber cellulosic nonwoven webs from a cellulose solution by melt blown technology and the products made thereby

Publications (1)

Publication Number Publication Date
US20050056956A1 true US20050056956A1 (en) 2005-03-17

Family

ID=34274283

Family Applications (1)

Application Number Title Priority Date Filing Date
US10/663,117 Abandoned US20050056956A1 (en) 2003-09-16 2003-09-16 Process for forming micro-fiber cellulosic nonwoven webs from a cellulose solution by melt blown technology and the products made thereby

Country Status (1)

Country Link
US (1) US20050056956A1 (en)

Cited By (72)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050079348A1 (en) * 2002-12-26 2005-04-14 Hyosung Corporation Lyocell multi-filament for tire cord and method of producing the same
US20070039704A1 (en) * 2005-08-22 2007-02-22 The Procter & Gamble Company Hydroxyl polymer fiber fibrous structures and processes for making same
US20070170609A1 (en) * 2004-11-10 2007-07-26 Hyosung Corporation Method for producing cellulose fiber
WO2007124522A1 (en) * 2006-04-28 2007-11-08 Lenzing Aktiengesellschaft Nonwoven melt-blown product
US20080015615A1 (en) * 2005-04-14 2008-01-17 Ethicon Endo-Surgery, Inc. Surgical clip advancement mechanism
US20080054516A1 (en) * 2004-12-30 2008-03-06 Ik-Hyun Kwon Method for Producing Cellulose Fiber
US20080169580A1 (en) * 2007-01-12 2008-07-17 Taiwan Textile Research Institute Apparatus and method for manufacturing non-woven fabric
WO2009009707A1 (en) * 2007-07-11 2009-01-15 E.I. Du Pont De Nemours And Company Infrared solvent stripping process
US20090022960A1 (en) * 2007-07-17 2009-01-22 Michael Donald Suer Fibrous structures and methods for making same
US20090023839A1 (en) * 2007-07-17 2009-01-22 Steven Lee Barnholtz Process for making fibrous structures
US20090022983A1 (en) * 2007-07-17 2009-01-22 David William Cabell Fibrous structures
US20090025894A1 (en) * 2007-07-17 2009-01-29 Steven Lee Barnholtz Fibrous structures and methods for making same
US20090026647A1 (en) * 2006-12-22 2009-01-29 Reifenhauser Gmbh & Co. Kg Maschinenfabrik Making a spunbond fleece from cellulosic filaments
US20090084513A1 (en) * 2007-07-17 2009-04-02 Steven Lee Barnholtz Fibrous structures and methods for making same
US20090186189A1 (en) * 2006-04-28 2009-07-23 Lenzing Aktiengesellschaft Hydroentangled Product Comprising Cellulose Fibers
US20090258562A1 (en) * 2008-04-11 2009-10-15 Biax Fiberfilm Process of forming a non-woven cellulose web and a web produced by said process
US20090256277A1 (en) * 2008-04-11 2009-10-15 Biax Fiberfilm Apparatus for extruding cellulose fibers
US20090258099A1 (en) * 2008-04-11 2009-10-15 Biax Fiberfilm Array of nozzles for extruding multiple cellulose fibers
US20100291823A1 (en) * 2008-01-11 2010-11-18 Lenzing Ag Microfiber
US20110037194A1 (en) * 2009-08-14 2011-02-17 Michael David James Die assembly and method of using same
US20110100574A1 (en) * 2009-11-02 2011-05-05 Steven Lee Barnholtz Fibrous structures that exhibit consumer relevant property values
US20110104970A1 (en) * 2009-11-02 2011-05-05 Steven Lee Barnholtz Low lint fibrous structures and methods for making same
EP2327817A1 (en) * 2009-11-27 2011-06-01 Japan Vilene Company, Ltd. Spinning apparatus and process for manufacturing nonwoven fabric
US20110177297A1 (en) * 2008-10-02 2011-07-21 Nurim Wellness Co. Ltd. Method of manufacturing solid microstructure and solid microstructure manufactured based on same
WO2012019035A2 (en) 2010-08-05 2012-02-09 Frank Scott Atchley Composite smokeless tobacco products, systems, and methods
KR101158553B1 (en) * 2008-12-30 2012-06-20 (주)엔티시 electric spinning apparatus
JP2013139655A (en) * 2012-01-05 2013-07-18 Teijin Ltd Nonwoven fabric of ultrafine diameter fiber and method for producing the same
US8608998B2 (en) 2008-07-09 2013-12-17 E I Du Pont De Nemours And Company Infrared solvent stripping process
US8641960B1 (en) * 2009-09-29 2014-02-04 The United States Of America, As Represented By The Secretary Of Agriculture Solution blow spinning
WO2014144013A1 (en) 2013-03-15 2014-09-18 Altria Client Services Inc. Pouch material for smokeless tobacco and tobacco substitute products
WO2014152956A1 (en) 2013-03-14 2014-09-25 Altria Client Services Inc. Product portion enrobing process and apparatus, and resulting products
US9066540B2 (en) 2010-08-05 2015-06-30 Altria Client Services Inc. Fabric having tobacco entangled with structural fibers
WO2015116766A1 (en) 2014-01-29 2015-08-06 Biax-Fiberfilm A high loft, nonwoven web exhibiting excellent recovery
CN104988586A (en) * 2015-07-21 2015-10-21 中国第一汽车股份有限公司 Porous material syringe needle-free static spinning apparatus
CN105200535A (en) * 2015-10-23 2015-12-30 天津市静海县远大工贸有限公司 Multi-row-hole spinning spraying head capable of greatly increasing production
US9303334B2 (en) 2014-05-07 2016-04-05 Biax-Fiberfilm Apparatus for forming a non-woven web
US9309612B2 (en) 2014-05-07 2016-04-12 Biax-Fiberfilm Process for forming a non-woven web
US9334592B2 (en) 2007-11-07 2016-05-10 Lenzing Aktiengesellschaft Process for the production of a hydroentangled product comprising cellulose fibers
US20160157978A1 (en) * 2014-12-05 2016-06-09 Ada Foundation Material deposition device and method of use
US9458573B2 (en) 2009-11-02 2016-10-04 The Procter & Gamble Company Fibrous structures and methods for making same
US9631321B2 (en) 2010-03-31 2017-04-25 The Procter & Gamble Company Absorptive fibrous structures
CN106968021A (en) * 2017-04-06 2017-07-21 超美斯新材料股份有限公司 A kind of high-efficient spinning device
US9896228B2 (en) 2014-03-14 2018-02-20 Altria Client Services Llc Polymer encased smokeless tobacco products
WO2018071928A1 (en) * 2016-10-21 2018-04-26 Lenzing Ag Process and device for the formation of directly-formed cellulosic webs
WO2018136895A1 (en) 2017-01-23 2018-07-26 Biax-Fiberfilm Corporation A high loft, nonwoven web exhibiting excellent recovery
EP3385427A1 (en) * 2017-04-03 2018-10-10 Lenzing Aktiengesellschaft Nonwoven cellulose fiber fabric with fiber diameter distribution
EP3385434A1 (en) * 2017-04-03 2018-10-10 Lenzing Aktiengesellschaft Nonwoven cellulose fiber fabric with merged fibers
WO2018184043A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven web designed for use in a clean room wipe
WO2018184047A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven web designed for use in a healthcare wiper
WO2018184049A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven material designed for use in hygiene applications
WO2018184041A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven web designed for use in a beauty face mask
WO2018184042A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven web designed for use in an industrial cleaning wipe
WO2018184038A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag Continuous filament cellulose nonwoven made with multiple bonding techniques
US10239089B2 (en) 2014-03-14 2019-03-26 Altria Client Services Llc Product portion enrobing process and apparatus
WO2019068764A1 (en) * 2017-10-06 2019-04-11 Lenzing Aktiengesellschaft Device for extruding filaments and producing spun-bonded fabrics
CN110079872A (en) * 2019-04-30 2019-08-02 上海化工研究院有限公司 A kind of preparation method of wide cut high-strength high-modulus polyethylene fiber
CN110582601A (en) * 2017-04-03 2019-12-17 兰精股份公司 cellulosic fiber nonwoven fabric with different aperture groups
EP3604652A1 (en) * 2018-07-31 2020-02-05 Lenzing Aktiengesellschaft Nonwoven fabric, use of the nonwoven fabric and wipe, dryer cloth and face mask containing the nonwoven fabric
US10633774B2 (en) 2014-05-07 2020-04-28 Biax-Fiberfilm Corporation Hybrid non-woven web and an apparatus and method for forming said web
US10704173B2 (en) 2014-01-29 2020-07-07 Biax-Fiberfilm Corporation Process for forming a high loft, nonwoven web exhibiting excellent recovery
CN111996674A (en) * 2020-08-18 2020-11-27 平湖爱之馨环保科技有限公司 Energy-saving equipment for preparing melt-blown fabric and method using equipment
US10895022B2 (en) 2009-11-02 2021-01-19 The Procter & Gamble Company Fibrous elements and fibrous structures employing same
US10961644B2 (en) 2014-01-29 2021-03-30 Biax-Fiberfilm Corporation High loft, nonwoven web exhibiting excellent recovery
WO2021094122A1 (en) 2019-11-13 2021-05-20 Deutsche Institute Für Textil- Und Faserforschung Denkendorf Nozzle device and manufacturing method for a nozzle device
WO2021122379A1 (en) 2019-12-17 2021-06-24 Lenzing Aktiengesellschaft Method for producing a spunbond nonwoven
WO2021170605A1 (en) * 2020-02-24 2021-09-02 Lenzing Aktiengesellschaft Method for producing spunbonded fabric
US20220049376A1 (en) * 2020-08-13 2022-02-17 Gelatex Technologies OÜ Device and method for producing polymer fibers and its uses thereof
CN114481451A (en) * 2020-10-28 2022-05-13 本田技研工业株式会社 Material layer forming apparatus
US11598026B2 (en) 2014-05-07 2023-03-07 Biax-Fiberfilm Corporation Spun-blown non-woven web
CN116334774A (en) * 2023-03-16 2023-06-27 扬州绿宝人造草坪有限公司 Melt spinning device for preparing artificial grass filaments
US11958308B1 (en) 2023-05-31 2024-04-16 G13 Innovation In Production Ltd Thermal paper, and methods and systems for forming the same
JP7477241B2 (en) 2018-07-31 2024-05-01 レンチング アクチエンゲゼルシャフト Nonwoven fabrics, uses of nonwoven fabrics, and wipes, dryer sheets, and face masks containing nonwoven fabrics

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2976580A (en) * 1953-07-16 1961-03-28 Riedel Johann Christoph Device for preparing a fleece, sliver or yarn, in particular of glass
US3689346A (en) * 1970-09-29 1972-09-05 Rowland Dev Corp Method for producing retroreflective material
US3709647A (en) * 1970-10-21 1973-01-09 Clear Pack Co Apparatus for forming an embossed thermoplastic sheet
US4552709A (en) * 1983-11-04 1985-11-12 The Procter & Gamble Company Process for high-speed production of webs of debossed and perforated thermoplastic film
US4931355A (en) * 1988-03-18 1990-06-05 Radwanski Fred R Nonwoven fibrous hydraulically entangled non-elastic coform material and method of formation thereof
US4960630A (en) * 1988-04-14 1990-10-02 International Paper Company Apparatus for producing symmetrical fluid entangled non-woven fabrics and related method
US5405650A (en) * 1992-04-03 1995-04-11 Johnson & Johnson Inc. Method for manufacturing a non-woven fabric marked with a print
US6230776B1 (en) * 1998-10-21 2001-05-15 Aaf International, Inc. Apparatus for forming fibrous filter media
US6358461B1 (en) * 1996-12-10 2002-03-19 Tencel Limited Method of manufacture of nonwoven fabric

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2976580A (en) * 1953-07-16 1961-03-28 Riedel Johann Christoph Device for preparing a fleece, sliver or yarn, in particular of glass
US3689346A (en) * 1970-09-29 1972-09-05 Rowland Dev Corp Method for producing retroreflective material
US3709647A (en) * 1970-10-21 1973-01-09 Clear Pack Co Apparatus for forming an embossed thermoplastic sheet
US4552709A (en) * 1983-11-04 1985-11-12 The Procter & Gamble Company Process for high-speed production of webs of debossed and perforated thermoplastic film
US4931355A (en) * 1988-03-18 1990-06-05 Radwanski Fred R Nonwoven fibrous hydraulically entangled non-elastic coform material and method of formation thereof
US4960630A (en) * 1988-04-14 1990-10-02 International Paper Company Apparatus for producing symmetrical fluid entangled non-woven fabrics and related method
US5405650A (en) * 1992-04-03 1995-04-11 Johnson & Johnson Inc. Method for manufacturing a non-woven fabric marked with a print
US6358461B1 (en) * 1996-12-10 2002-03-19 Tencel Limited Method of manufacture of nonwoven fabric
US6230776B1 (en) * 1998-10-21 2001-05-15 Aaf International, Inc. Apparatus for forming fibrous filter media

Cited By (170)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050079348A1 (en) * 2002-12-26 2005-04-14 Hyosung Corporation Lyocell multi-filament for tire cord and method of producing the same
US20070170609A1 (en) * 2004-11-10 2007-07-26 Hyosung Corporation Method for producing cellulose fiber
US20080054516A1 (en) * 2004-12-30 2008-03-06 Ik-Hyun Kwon Method for Producing Cellulose Fiber
US20080015615A1 (en) * 2005-04-14 2008-01-17 Ethicon Endo-Surgery, Inc. Surgical clip advancement mechanism
US8921244B2 (en) 2005-08-22 2014-12-30 The Procter & Gamble Company Hydroxyl polymer fiber fibrous structures and processes for making same
US20070039704A1 (en) * 2005-08-22 2007-02-22 The Procter & Gamble Company Hydroxyl polymer fiber fibrous structures and processes for making same
US8282877B2 (en) 2006-04-28 2012-10-09 Lenzing Aktiengesellschaft Process of making a hydroentangled product from cellulose fibers
WO2007124522A1 (en) * 2006-04-28 2007-11-08 Lenzing Aktiengesellschaft Nonwoven melt-blown product
US20090312731A1 (en) * 2006-04-28 2009-12-17 Lenzing Aktiengesellschaft Nonwoven Melt-Blown Product
US20090186189A1 (en) * 2006-04-28 2009-07-23 Lenzing Aktiengesellschaft Hydroentangled Product Comprising Cellulose Fibers
US20090026647A1 (en) * 2006-12-22 2009-01-29 Reifenhauser Gmbh & Co. Kg Maschinenfabrik Making a spunbond fleece from cellulosic filaments
US20080169580A1 (en) * 2007-01-12 2008-07-17 Taiwan Textile Research Institute Apparatus and method for manufacturing non-woven fabric
WO2009009707A1 (en) * 2007-07-11 2009-01-15 E.I. Du Pont De Nemours And Company Infrared solvent stripping process
US20090022983A1 (en) * 2007-07-17 2009-01-22 David William Cabell Fibrous structures
US11639581B2 (en) 2007-07-17 2023-05-02 The Procter & Gamble Company Fibrous structures and methods for making same
US20090084513A1 (en) * 2007-07-17 2009-04-02 Steven Lee Barnholtz Fibrous structures and methods for making same
US20090025894A1 (en) * 2007-07-17 2009-01-29 Steven Lee Barnholtz Fibrous structures and methods for making same
US11346056B2 (en) 2007-07-17 2022-05-31 The Procter & Gamble Company Fibrous structures and methods for making same
US8852474B2 (en) 2007-07-17 2014-10-07 The Procter & Gamble Company Process for making fibrous structures
US20090022960A1 (en) * 2007-07-17 2009-01-22 Michael Donald Suer Fibrous structures and methods for making same
WO2009010940A2 (en) * 2007-07-17 2009-01-22 The Procter & Gamble Company Process for making fibrous structures
US20090023839A1 (en) * 2007-07-17 2009-01-22 Steven Lee Barnholtz Process for making fibrous structures
US9926648B2 (en) 2007-07-17 2018-03-27 The Procter & Gamble Company Process for making fibrous structures
US11414798B2 (en) 2007-07-17 2022-08-16 The Procter & Gamble Company Fibrous structures
US10858785B2 (en) 2007-07-17 2020-12-08 The Procter & Gamble Company Fibrous structures and methods for making same
US11959225B2 (en) 2007-07-17 2024-04-16 The Procter & Gamble Company Fibrous structures and methods for making same
WO2009010940A3 (en) * 2007-07-17 2009-03-12 Procter & Gamble Process for making fibrous structures
US7972986B2 (en) 2007-07-17 2011-07-05 The Procter & Gamble Company Fibrous structures and methods for making same
US10024000B2 (en) 2007-07-17 2018-07-17 The Procter & Gamble Company Fibrous structures and methods for making same
US20110209840A1 (en) * 2007-07-17 2011-09-01 Steven Lee Barnholtz Fibrous structures and methods for making same
US10513801B2 (en) 2007-07-17 2019-12-24 The Procter & Gamble Company Process for making fibrous structures
US9334592B2 (en) 2007-11-07 2016-05-10 Lenzing Aktiengesellschaft Process for the production of a hydroentangled product comprising cellulose fibers
US11932969B2 (en) 2008-01-11 2024-03-19 Lenzing Aktiengesellschaft Microfiber
US20100291823A1 (en) * 2008-01-11 2010-11-18 Lenzing Ag Microfiber
US8029259B2 (en) 2008-04-11 2011-10-04 Reifenhauser Gmbh & Co. Kg Maschinenfabrik Array of nozzles for extruding multiple cellulose fibers
US8029260B2 (en) 2008-04-11 2011-10-04 Reifenhauser Gmbh & Co. Kg Maschinenfabrik Apparatus for extruding cellulose fibers
US8303888B2 (en) 2008-04-11 2012-11-06 Reifenhauser Gmbh & Co. Kg Process of forming a non-woven cellulose web and a web produced by said process
US20090258099A1 (en) * 2008-04-11 2009-10-15 Biax Fiberfilm Array of nozzles for extruding multiple cellulose fibers
US20090256277A1 (en) * 2008-04-11 2009-10-15 Biax Fiberfilm Apparatus for extruding cellulose fibers
US20090258562A1 (en) * 2008-04-11 2009-10-15 Biax Fiberfilm Process of forming a non-woven cellulose web and a web produced by said process
US8608998B2 (en) 2008-07-09 2013-12-17 E I Du Pont De Nemours And Company Infrared solvent stripping process
JP2012504034A (en) * 2008-10-02 2012-02-16 ヌリ−エム ウェルネス カンパニー リミテッド Manufacturing method of solid microstructure by air blowing and solid microstructure manufactured therefrom
US20110177297A1 (en) * 2008-10-02 2011-07-21 Nurim Wellness Co. Ltd. Method of manufacturing solid microstructure and solid microstructure manufactured based on same
KR101158553B1 (en) * 2008-12-30 2012-06-20 (주)엔티시 electric spinning apparatus
US10704166B2 (en) * 2009-08-14 2020-07-07 The Procter & Gamble Company Die assembly and method of using same
US11414787B2 (en) 2009-08-14 2022-08-16 The Procter & Gamble Company Die assembly and methods of using same
US20110037194A1 (en) * 2009-08-14 2011-02-17 Michael David James Die assembly and method of using same
US11739444B2 (en) 2009-08-14 2023-08-29 The Procter & Gamble Company Die assembly and methods of using same
US8641960B1 (en) * 2009-09-29 2014-02-04 The United States Of America, As Represented By The Secretary Of Agriculture Solution blow spinning
US20110104970A1 (en) * 2009-11-02 2011-05-05 Steven Lee Barnholtz Low lint fibrous structures and methods for making same
US10895022B2 (en) 2009-11-02 2021-01-19 The Procter & Gamble Company Fibrous elements and fibrous structures employing same
US20110100574A1 (en) * 2009-11-02 2011-05-05 Steven Lee Barnholtz Fibrous structures that exhibit consumer relevant property values
US9714484B2 (en) 2009-11-02 2017-07-25 The Procter & Gamble Company Fibrous structures and methods for making same
US9458573B2 (en) 2009-11-02 2016-10-04 The Procter & Gamble Company Fibrous structures and methods for making same
US11618977B2 (en) 2009-11-02 2023-04-04 The Procter & Gamble Company Fibrous elements and fibrous structures employing same
EP2327817A1 (en) * 2009-11-27 2011-06-01 Japan Vilene Company, Ltd. Spinning apparatus and process for manufacturing nonwoven fabric
US20110130063A1 (en) * 2009-11-27 2011-06-02 Japan Vilene Company, Ltd. Spinning apparatus, apparatus and process for manufacturing nonwoven fabric, and nonwoven fabric
US10240297B2 (en) 2010-03-31 2019-03-26 The Procter & Gamble Company Fibrous structures and methods for making same
US9631321B2 (en) 2010-03-31 2017-04-25 The Procter & Gamble Company Absorptive fibrous structures
US11680373B2 (en) 2010-03-31 2023-06-20 The Procter & Gamble Company Container for fibrous wipes
US10697127B2 (en) 2010-03-31 2020-06-30 The Procter & Gamble Company Fibrous structures and methods for making same
US10448669B2 (en) 2010-08-05 2019-10-22 Altria Client Services Llc Non-tobacco product having polyurethane structural fibers
WO2012019035A2 (en) 2010-08-05 2012-02-09 Frank Scott Atchley Composite smokeless tobacco products, systems, and methods
US11540560B2 (en) 2010-08-05 2023-01-03 Altria Client Services Llc Fabric having tobacco entangled with structural fibers
US9756875B2 (en) 2010-08-05 2017-09-12 Altria Client Services Llc Composite smokeless tobacco products, systems, and methods
US9066540B2 (en) 2010-08-05 2015-06-30 Altria Client Services Inc. Fabric having tobacco entangled with structural fibers
US8978661B2 (en) 2010-08-05 2015-03-17 Altria Client Services Inc. Composite smokeless tobacco products, systems, and methods
US9814261B2 (en) 2010-08-05 2017-11-14 Altria Client Services Llc Fabric having tobacco entangled with structural fibers
US10736354B2 (en) 2010-08-05 2020-08-11 Altria Client Services Llc Fabric having tobacco entangled with structural fibers
JP2013139655A (en) * 2012-01-05 2013-07-18 Teijin Ltd Nonwoven fabric of ultrafine diameter fiber and method for producing the same
US9763473B2 (en) 2013-03-14 2017-09-19 Altria Client Services Llc Fiber-wrapped smokeless tobacco product
WO2014152956A1 (en) 2013-03-14 2014-09-25 Altria Client Services Inc. Product portion enrobing process and apparatus, and resulting products
US11103002B2 (en) 2013-03-14 2021-08-31 Altria Client Services Llc Product portion enrobing machines and methods
US10905151B2 (en) 2013-03-14 2021-02-02 Altria Client Services Llc Fiber-wrapped smokeless tobacco product
US11382350B2 (en) 2013-03-14 2022-07-12 Altria Client Services Llc Product portion enrobing process and apparatus, and resulting products
WO2014152938A1 (en) 2013-03-14 2014-09-25 Altria Client Services Inc. Product portion enrobing machines and methods
US11889857B2 (en) 2013-03-14 2024-02-06 Altria Client Services Llc Product portion enrobing machines and methods
WO2014152945A1 (en) 2013-03-14 2014-09-25 Altria Client Services Inc. Fiber-wrapped smokeless-tobacco product
US10588339B2 (en) 2013-03-14 2020-03-17 Altria Client Services Llc Product portion enrobing machines and methods
US10531685B2 (en) 2013-03-14 2020-01-14 Altria Client Services Llc Product portion enrobing process and apparatus, and resulting products
US9414624B2 (en) 2013-03-14 2016-08-16 Altria Client Services Llc Fiber-wrapped smokeless tobacco product
US9462827B2 (en) 2013-03-14 2016-10-11 Altria Client Services Llc Product portion enrobing process and apparatus, and resulting products
US11723394B2 (en) 2013-03-14 2023-08-15 Altria Client Services Llc Fiber-wrapped smokeless tobacco product
US10306916B2 (en) 2013-03-14 2019-06-04 Altria Client Services Llc Product portion enrobing machines and methods
EP4218429A2 (en) 2013-03-14 2023-08-02 Altria Client Services LLC Fiber-wrapped smokeless-tobacco product
US10258076B2 (en) 2013-03-14 2019-04-16 Altria Client Services Llc Fiber-wrapped smokeless tobacco product
US20170208854A1 (en) 2013-03-14 2017-07-27 Altria Client Services Llc Product Portion Enrobing Process and Apparatus, and Resulting Products
US9693582B2 (en) 2013-03-14 2017-07-04 Altria Client Services Llc Product portion enrobing machines and methods
US11375740B2 (en) 2013-03-15 2022-07-05 Altria Client Services Llc Methods and machines for pouching smokeless tobacco and tobacco substitute products
US10039309B2 (en) 2013-03-15 2018-08-07 Altria Client Services Llc Pouch material for smokeless tobacco and tobacco substitute products
EP4154736A1 (en) 2013-03-15 2023-03-29 Altria Client Services LLC Methods and machines for pouching smokeless tobacco and tobacco substitute products
WO2014144013A1 (en) 2013-03-15 2014-09-18 Altria Client Services Inc. Pouch material for smokeless tobacco and tobacco substitute products
US11882866B2 (en) 2013-03-15 2024-01-30 Altria Client Services Llc Pouch material for smokeless tobacco and tobacco substitute products
US10765142B2 (en) 2013-03-15 2020-09-08 Altria Client Services Llc Methods and machines for pouching smokeless tobacco and tobacco substitute products
US10028521B2 (en) 2013-03-15 2018-07-24 Altria Client Services Llc Methods and machines for pouching smokeless tobacco and tobacco substitute products
US10463070B2 (en) 2013-03-15 2019-11-05 Altria Client Services Llc Pouch material for smokeless tobacco and tobacco substitute products
US11000060B2 (en) 2013-03-15 2021-05-11 Altria Client Services Llc Pouch material for smokeless tobacco and tobacco substitute products
WO2014144254A2 (en) 2013-03-15 2014-09-18 Altria Client Services Inc. Methods and machines for pouching smokeless tobacco and tobacco substitute products
US11284643B2 (en) 2013-03-15 2022-03-29 Altria Client Services Llc Methods and machines for pouching smokeless tobacco and tobacco substitute products
US10813382B2 (en) 2013-03-15 2020-10-27 Altria Client Services Llc Methods and machines for pouching smokeless tobacco and tobacco substitute products
US11812776B2 (en) 2013-03-15 2023-11-14 Altria Client Services Llc Methods and machines for pouching smokeless tobacco and tobacco substitute products
US10704173B2 (en) 2014-01-29 2020-07-07 Biax-Fiberfilm Corporation Process for forming a high loft, nonwoven web exhibiting excellent recovery
US10961644B2 (en) 2014-01-29 2021-03-30 Biax-Fiberfilm Corporation High loft, nonwoven web exhibiting excellent recovery
WO2015116766A1 (en) 2014-01-29 2015-08-06 Biax-Fiberfilm A high loft, nonwoven web exhibiting excellent recovery
US10875051B2 (en) 2014-03-14 2020-12-29 Altria Client Services Llc Product portion enrobing process and apparatus
EP3597052A1 (en) 2014-03-14 2020-01-22 Altria Client Services LLC Product portion enrobing process and apparatus
US11198151B2 (en) 2014-03-14 2021-12-14 Altria Client Services Llc Polymer encased smokeless tobacco products
US9896228B2 (en) 2014-03-14 2018-02-20 Altria Client Services Llc Polymer encased smokeless tobacco products
US10384816B2 (en) 2014-03-14 2019-08-20 Altria Client Services Llc Polymer encased smokeless tobacco products
US11731162B2 (en) 2014-03-14 2023-08-22 Altria Client Services Llc Polymer encased smokeless tobacco products
US10239089B2 (en) 2014-03-14 2019-03-26 Altria Client Services Llc Product portion enrobing process and apparatus
US11598026B2 (en) 2014-05-07 2023-03-07 Biax-Fiberfilm Corporation Spun-blown non-woven web
US9309612B2 (en) 2014-05-07 2016-04-12 Biax-Fiberfilm Process for forming a non-woven web
US10633774B2 (en) 2014-05-07 2020-04-28 Biax-Fiberfilm Corporation Hybrid non-woven web and an apparatus and method for forming said web
US9303334B2 (en) 2014-05-07 2016-04-05 Biax-Fiberfilm Apparatus for forming a non-woven web
US9775694B2 (en) * 2014-12-05 2017-10-03 American Dental Association Foundation Material deposition device and method of use
US20160157978A1 (en) * 2014-12-05 2016-06-09 Ada Foundation Material deposition device and method of use
CN104988586A (en) * 2015-07-21 2015-10-21 中国第一汽车股份有限公司 Porous material syringe needle-free static spinning apparatus
CN105200535A (en) * 2015-10-23 2015-12-30 天津市静海县远大工贸有限公司 Multi-row-hole spinning spraying head capable of greatly increasing production
WO2018071928A1 (en) * 2016-10-21 2018-04-26 Lenzing Ag Process and device for the formation of directly-formed cellulosic webs
US11767623B2 (en) * 2016-10-21 2023-09-26 Lenzing Ag Process and device for the formation of directly-formed cellulosic webs
US11371173B2 (en) * 2016-10-21 2022-06-28 Lenzing Ag Process and device for the formation of directly-formed cellulosic webs
US20220364282A1 (en) * 2016-10-21 2022-11-17 Lenzing Ag Process and device for the formation of directly-formed cellulosic webs
JP2019532194A (en) * 2016-10-21 2019-11-07 レンチング アクチエンゲゼルシャフト Method and apparatus for forming directly formed cellulosic webs
JP7091580B2 (en) 2016-10-21 2022-06-28 レンチング アクチエンゲゼルシャフト Methods and equipment for forming directly formed cellulosic webs
TWI765921B (en) * 2016-10-21 2022-06-01 奧地利商蘭仁股份有限公司 Process and device for the formation of directly formed cellulosic webs
KR102436366B1 (en) 2016-10-21 2022-08-25 렌징 악티엔게젤샤프트 Methods and Apparatus for Forming Direct Forming Cellulosic Webs
KR20190066064A (en) * 2016-10-21 2019-06-12 렌징 악티엔게젤샤프트 Method and apparatus for the formation of directly formed cellulosic webs
CN109844202A (en) * 2016-10-21 2019-06-04 连津格股份公司 It is used to form the process and equipment of the cellulose mesh directly formed
RU2757398C2 (en) * 2016-10-21 2021-10-15 Ленцинг Аг Method and device for forming cellulose canvas by direct molding
AT519489B1 (en) * 2016-10-21 2021-11-15 Chemiefaser Lenzing Ag Method and apparatus for producing cellulose-based nonwovens which are formed directly from Lyocell spinning solution
WO2018136895A1 (en) 2017-01-23 2018-07-26 Biax-Fiberfilm Corporation A high loft, nonwoven web exhibiting excellent recovery
WO2018184042A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven web designed for use in an industrial cleaning wipe
WO2018184049A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven material designed for use in hygiene applications
EP3385427A1 (en) * 2017-04-03 2018-10-10 Lenzing Aktiengesellschaft Nonwoven cellulose fiber fabric with fiber diameter distribution
KR102298010B1 (en) * 2017-04-03 2021-09-03 렌징 악티엔게젤샤프트 Continuous filament cellulosic nonwoven fabric made by multiple bonding techniques
EP3385434A1 (en) * 2017-04-03 2018-10-10 Lenzing Aktiengesellschaft Nonwoven cellulose fiber fabric with merged fibers
WO2018184043A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven web designed for use in a clean room wipe
WO2018184047A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven web designed for use in a healthcare wiper
WO2018184941A1 (en) * 2017-04-03 2018-10-11 Lenzing Aktiengesellschaft Nonwoven cellulose fiber fabric with merged fibers
WO2018184937A1 (en) * 2017-04-03 2018-10-11 Lenzing Aktiengesellschaft Nonwoven cellulose fiber fabric with fiber diameter distribution
WO2018184041A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag A nonwoven web designed for use in a beauty face mask
WO2018184038A1 (en) * 2017-04-03 2018-10-11 Lenzing Ag Continuous filament cellulose nonwoven made with multiple bonding techniques
KR20190127975A (en) * 2017-04-03 2019-11-13 렌징 악티엔게젤샤프트 Continuous filament cellulose nonwovens made by multiple bonding techniques
CN110506139A (en) * 2017-04-03 2019-11-26 连津格股份公司 The continuous filament fibers element non-woven cloth made of a variety of adhering techniques
JP2020513072A (en) * 2017-04-03 2020-04-30 レンツィング アクツィエンゲゼルシャフト Non-woven cellulose fiber cloth having fiber diameter distribution
US11613097B2 (en) * 2017-04-03 2023-03-28 Lenzing Ag Continuous filament cellulose nonwoven made with multiple bonding techniques
TWI788337B (en) * 2017-04-03 2023-01-01 奧地利商蘭仁股份有限公司 Nonwoven cellulose fiber fabric, method and device for manufacturing the same, method of using the same, and product comprising the same
CN110582601A (en) * 2017-04-03 2019-12-17 兰精股份公司 cellulosic fiber nonwoven fabric with different aperture groups
CN106968021A (en) * 2017-04-06 2017-07-21 超美斯新材料股份有限公司 A kind of high-efficient spinning device
JP2020536180A (en) * 2017-10-06 2020-12-10 レンチング アクチエンゲゼルシャフト Equipment for extruding filaments and producing spunbonded fabrics
US20200291545A1 (en) * 2017-10-06 2020-09-17 Lenzing Aktiengesellschaft Device for the Extrusion of Filaments and for the Production of Spunbonded Fabrics
JP7282083B2 (en) 2017-10-06 2023-05-26 レンチング アクチエンゲゼルシャフト Equipment for extruding filaments and producing spunbond fabrics
WO2019068764A1 (en) * 2017-10-06 2019-04-11 Lenzing Aktiengesellschaft Device for extruding filaments and producing spun-bonded fabrics
CN111194363A (en) * 2017-10-06 2020-05-22 连津格股份公司 Apparatus for extrusion and production of spun-bonded fabrics from filaments
WO2020025440A1 (en) * 2018-07-31 2020-02-06 Lenzing Aktiengesellschaft Nonwoven material, use of the nonwoven material, and wiping cloth, drying cloth and face mask containing the nonwoven material
JP2021533280A (en) * 2018-07-31 2021-12-02 レンチング アクチエンゲゼルシャフト Non-woven fabrics, use of non-woven fabrics, and wipes containing non-woven fabrics, dryer sheets, and face masks.
JP7477241B2 (en) 2018-07-31 2024-05-01 レンチング アクチエンゲゼルシャフト Nonwoven fabrics, uses of nonwoven fabrics, and wipes, dryer sheets, and face masks containing nonwoven fabrics
EP3604652A1 (en) * 2018-07-31 2020-02-05 Lenzing Aktiengesellschaft Nonwoven fabric, use of the nonwoven fabric and wipe, dryer cloth and face mask containing the nonwoven fabric
CN112513357A (en) * 2018-07-31 2021-03-16 连津格股份公司 Nonwoven fabric, use of nonwoven fabric, and wipe, paper for drying, and mask containing the nonwoven fabric
CN110079872A (en) * 2019-04-30 2019-08-02 上海化工研究院有限公司 A kind of preparation method of wide cut high-strength high-modulus polyethylene fiber
WO2021094122A1 (en) 2019-11-13 2021-05-20 Deutsche Institute Für Textil- Und Faserforschung Denkendorf Nozzle device and manufacturing method for a nozzle device
WO2021122379A1 (en) 2019-12-17 2021-06-24 Lenzing Aktiengesellschaft Method for producing a spunbond nonwoven
WO2021170605A1 (en) * 2020-02-24 2021-09-02 Lenzing Aktiengesellschaft Method for producing spunbonded fabric
US11697892B2 (en) * 2020-08-13 2023-07-11 Gelatex Technologies OÜ Device and method for producing polymer fibers and its uses thereof
US20220049376A1 (en) * 2020-08-13 2022-02-17 Gelatex Technologies OÜ Device and method for producing polymer fibers and its uses thereof
CN111996674A (en) * 2020-08-18 2020-11-27 平湖爱之馨环保科技有限公司 Energy-saving equipment for preparing melt-blown fabric and method using equipment
CN114481451A (en) * 2020-10-28 2022-05-13 本田技研工业株式会社 Material layer forming apparatus
CN116334774A (en) * 2023-03-16 2023-06-27 扬州绿宝人造草坪有限公司 Melt spinning device for preparing artificial grass filaments
US11958308B1 (en) 2023-05-31 2024-04-16 G13 Innovation In Production Ltd Thermal paper, and methods and systems for forming the same

Similar Documents

Publication Publication Date Title
US20050056956A1 (en) Process for forming micro-fiber cellulosic nonwoven webs from a cellulose solution by melt blown technology and the products made thereby
WO2005106085A1 (en) Apparatus , product and process forming micro-fiber cellulosic nonwoven webs
US11767623B2 (en) Process and device for the formation of directly-formed cellulosic webs
US8241024B2 (en) Forming melt spun nonwowen webs
KR100987743B1 (en) Method and device for the manufacture of a spunbonded fabric of cellulosic filaments
KR101637620B1 (en) A nonwoven composite and method for making the same
US20080023873A1 (en) Process for Preparing a Non-Woven Cellulosic Structure and the Non-Woven Cellulosic Structure Prepared Therefrom
EP1896635B1 (en) Method for the production of nonwoven fabrics
US20080220161A1 (en) Method of and apparatus for making a spunbond
KR19980701273A (en) MANUFACTURE OF EXTRUDED ATRICLES
KR100492069B1 (en) Process and device for the transport of continuous moldings without tensile stress
KR20220010547A (en) Method and apparatus for cleaning spinnerettes in the manufacture of cellulose-based spunbond nonwovens
WO2018184046A1 (en) A nonwoven material designed for use as filter media
US20100159774A1 (en) Nonwoven composite and method for making the same
EP1024940A1 (en) Method and apparatus for in-line splitting of plural-component fibers and formation of nonwoven fabrics
CN215800077U (en) Splitting type crimped spun-bonded filament production equipment and non-woven fabric production line comprising same
CN115182096B (en) Cellulose filament non-woven material and preparation method thereof
CN115182097A (en) Cellulose filament non-woven material production device
CN217809926U (en) Cellulose filament non-woven material production device
US20230051927A1 (en) Process for the production of spunbonded nonwoven
KR20220111706A (en) Manufacturing method of spunbonded nonwoven fabric

Legal Events

Date Code Title Description
AS Assignment

Owner name: BIAX FIBERFILM CORPORATION, WISCONSIN

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:ZHAO, RONGGUO;REEL/FRAME:016628/0758

Effective date: 20050319

STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION