US3842151A - Method for preparing fibers from polymer solutions - Google Patents

Method for preparing fibers from polymer solutions Download PDF

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Publication number
US3842151A
US3842151A US00316006A US31600672A US3842151A US 3842151 A US3842151 A US 3842151A US 00316006 A US00316006 A US 00316006A US 31600672 A US31600672 A US 31600672A US 3842151 A US3842151 A US 3842151A
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solvent
gaseous medium
spinneret
polymer solution
solution
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V Stoy
J Prokop
R Urbanova
A Stoy
J Kucera
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Czech Academy of Sciences CAS
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Czech Academy of Sciences CAS
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    • 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
    • D01D5/06—Wet spinning methods
    • 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
    • D01D5/04—Dry spinning methods

Definitions

  • the present invention relates to a method and apparatus for treating polymer solutions to form fibers, strings, chords, tubings, films, etc. and particularly to a method and apparatus combining the advantages of dry and wet spinning.
  • Polymer solutions are usually spun to form fibers elther by the dry or by the wet method.
  • fibers all fiber-like articles having lateral dimension much smaller than the length are, for brevity sake, called fibers.
  • the dry spinning consists in extruding the poly mer solution through a spinneret into a heated tubular shaft, where the solvent evaporates gradually, so that a substantially dry fiber exits from the bottom of the shaft.
  • An additional step in which the fiber is washed is sometimes included, because the last traces of solvent are very diflicult to remove in the atmosphere of the shaft.
  • Wet spinning consists generally in extruding a polymer solution through a spinneret into a coagulation bath, where the polymer hardens and the solvent is washed off with a suitable liquid, e.g. with water. In this way thermal strain on the fiber does not occur, and the coagulation path is shorter than the atmospheric dry shaft.
  • solutions of polymers in non-volatile solvents can be treated by this method, as for example, polyacrylonitrile dissolved in concentrated aqueous zinc chloride or sodium rhodanide solution, proteins or cellulose xanthate in alkalineous solutions, etc.
  • the solvents used need to be recovered from more or less diluted solutions, and the concentration of the polymer in the spun solution and spinning velocity are rather low, so that the output of a wet device is usually several times smaller than that of a device for dry spinning, of the same size.
  • the extruded polymer solution leaves the spinneret forming a jet streaming through a surrounding fluid medium.
  • the solvent penetrates by diffusion from the solution into the gaseous or liquid surrounding medium. If the diflz'usion into the liquid surrounding is very fast, a skin consisting of a coagulated, more or less plasticized polymer is formed on the surface of the polymer stream. The skin obstructs further diffusion and the entirety works as an osmotic cell due to the fact that the molecules of the solvent and those of the precipitant have a difierent size.
  • the molecules of the solvent are usually more bulky, so that the precipitant (such as water) penetrates more rapidly into the spun stream of the polymer than the rate at which the solvent can diifuse outwardly.
  • microvoids occur in the structure of the resultant filament causing crimps, i.e. heterogeneous structure with poor mechanical properties.
  • Coagulation must be carried out gently and slowly in order that the loss of solvent concentrated on the surface layer of the jet stream could occur only by diffusion from its inner parts.
  • the coagulation rate must be reduced, e.g. by reducing the temperature of the coagulation bath, or by coagulating the fiber in several successive baths with gradually increasing concentration of the precipitation agent.
  • the polymer cannot be in a concentration which is too high.
  • Another factor limiting the spinning velocity is the splashing of the coagulation liquid by the movement of the filament and the rollers (galettes) at high drawing-off velocities, and the hydrodynamic resistance of the coagulation bath to the stream of the polymer solution before it solidified, resulting in diminishing the diameter of the polymer stream and sometimes even in its interruption.
  • the present invention comprises the steps of sequentially and in a continuous manner extrcding a polymer solution into a gaseous or dry atmosphere maintained at a pressure below ambient atmospheric pressure and thereafter passing the extrusion through at least one coagulating bath.
  • a polymer solution is extruded through a spinneret into a tube or shaft, which is on its upper end and sealed against gas fiow by a lid connected with the said spinnerett, and its lower end is placed below the level of a suitable coagulation bath, open to atmosphere.
  • Pressure within the tube, between the spinneret and the level of the coagulation bath is maintained lower than the pressure outside the shaft, so that the level of the coagulation liquid is higher in the shaft than in the outer coagulation bath.
  • FIG. 1 is a schematic side view of extruding apparatus and dry and wet coagulation apparatus according to the present invention
  • FIG. 2 is a view similar to that of FIG. 1 showing the means for circulating the coagulating liquid, and for maintaining the necessary pressure level in the system;
  • FIG. 3 is a view similar to that of FIG. 2 showing the gas circulation system
  • FIG. 4 is a view showing an alternative embodiment for the apparatus of FIG. 1.
  • polymer solutions is intended to cover all polymers, copolymers, and mixtures, in solutions, suitable for the production of fibers, filaments, etc. by the coagulation techniques in dry or Wet system. Specific disclosures of all polymer solutions are not believed necessary since they do not per-se form a part of this invention.
  • the method of the present invention may be best exemplified by reference to the basic arrangement as seen in FIG. 1.
  • the polymer solution 1 e.g. polyacrylonitrile dissolved in 65% nitric acid
  • the solution forms a stream in a shape of the fiber 3 passing through the space 6 between the spinneret 2 and a coagulation liquid 5 is open to atmosphere.
  • the space 6 is limited by the body of the shaft 4.
  • the pressure of the gas in the space 6 is reduced by means of vacuum forming attachment 7 which sucks off the liquid in bath 5, so that the level of the coagulation liquid can be elevated on any desired height and kept there.
  • the stream of the polymer solution 3 proceeds in the space 6 through a flow of a gaseous medium, which may, if desired, be heated, and which is preferably led counter-currentwise to the movement of the stream.
  • the gas is led into the space 6 through an intake port 8, situated above the level of the liquid 5, and out through the outlet port 9, situated below the fixed spinneret.
  • the spinneret seals the upper end of the space 6 in gas-tight condition.
  • the evaporation in space 6 of the solvent from the surface layer causes the formation of a skin on the fiber filament, which retards the more rapid diffusion of the solvent.
  • a homogeneous fiber may be formed even if the coagulation is rather swift.
  • the result is similar to that of the spinning of a polymer solution having a higher viscosity.
  • the viscosity of the solution is, in practice, limited since the hydrodynamic resistance in the spinneret places restraints on it.
  • undesirable viscoelastic effects occur just below the opening of the spinneret.
  • the reduced pressure below the spinneret helps in the extruding of the solution, so that the actual spinning pressure exerted by the piston may be lower.
  • the skin formed by the rapid evaporation of at least a portion of the sol vent from the surface of the polymer solution jet stream provides mechanical strength, so that the stream cannot be broken or interrupted due to the viscoelastic effects.
  • the advantage of the method according to the present invention is that the solvent evaporates at a reduced pressure and thus the fiber undergoes less thermal strain.
  • the rate of the evaporation can be controlled not only by the supply of heat to the gas and by the countercurrent flow of the gaseous medium in the space 6, but also by the retention of the solvent vapors in this space.
  • the saturation of gas with solvent can be thus controlled more readily than in usual open shaft, and polymer solutions even being very volatile solvents (such as methylene chloride), can be spun.
  • the solutions are otherwise not suitable for the dry spinning due to their excessive volatility.
  • the solvent may be recovered from the gas in a completely closed circuit, reducing substantially the loss of solvent.
  • the spinning device itself is much shorter than the usual apparatus and the last traces of the solvent, which can not be easily removed by evaporation can be washed off in the coagulation bath rather than extending the shaft indefinitely.
  • the present invention utilizes the dry spinning at the first stage of the coagulation, and the wet method at the second stage, both in the conditions, where their virtues can be utilized most advantageously. Accordingly even a bicomponent fiber can be produced besides the common homogeneous fiber and such fibers can be permanently crimped by suitable aftertreatment, eg by the stretching and the stabilization.
  • the apparatus of FIG. 1 is provided with a split spinneret, each part charged with a polymer solution of diiferent properties feeding into each part of the orifice.
  • the method of forming crimped bicomponent fibers through a split spinneret is well known as such, but its combination with the method according to our invention provides numerous advantages.
  • a spinneret with rather large orifices can be used.
  • the diameter of the orifice may be much larger than that of the fiber formed, snice the latter can be diminished by stretching the polymer solution jet before it meets the interface of the coagulation liquid.
  • the bicomponent fiber made by hitherto known methods often tends to split longitudinally into two parts, because both solutions meeting each other in the orifice do not have enough time to mutually penetrate into each other to an extent sufficient to form a lasting joint.
  • the enthalpy or pressure/heat conditions for evaporation of the solvent can be supplied either by heating the gaseous medium supplied to space 6, by recycling the gas below the spinneret, by radiant heating of the shaft (e.g. by means of heating elements in the wall of the shaft), or by means of a heated spinneret.
  • the advantage of the latter is that viscosity of the solution decreases due to the elevated temperature only in the smallest hydrodynamic cross-section, so that it is possible to use higher concentration of the polymer in the solution, or to raise the spinning velocity without resulting in the mentioned undesirable viscoelastic effects, or the need to apply a lower pressure by the piston before the spinneret.
  • the low pressure beneath the spinneret permits the use of less heat and a lower temperature in the space 6.
  • the amount of the applied enthalpy must not be too large, since the polymer solution is often not sufficiently thermo-stabile, and it may decompose if it were.
  • the solvent must not boil when the solution comes into the space 6 having the reduced pressure.
  • the resultant bubbles of the boiling solvent vapor would cause the breaking and interruption of the filament. That is why it is most advantageous to supply a major part of the heat to the space 6 below the spinneret, and over a path as long as possible. This can be easily done by heating the gaseous medium itself before entry and/or by infrared irradiation on the length of the cylinder 4.
  • the fiber pre-formed in space 6 mets the coagulation liquid 5 more of the solvent Washes off and the fiber further solidifies and hardens.
  • the hardened fiber is drawn off via galette to a further washing, elongation, shape stabilization and reeling apparatus.
  • the coagulation rate must be necessarily limited to a reasonable value, for otherwise a heterogeneous fiber having bad mechanical properties may be formed. For this reason it is preferred to use a suitable technological measure to prevent rapid coagulation.
  • the fiber may be led through an array of baths, each having a gradually increasing concentration of the precipitation agent and gradually decreasing concentration of the solvent.
  • the shape of the vessel holding coagulation bath 5 may be L-shaped. Such a shape does not take much room either in the vertical, or in the horizontal direction. Also the over-all volume of the bath may be smaller than that of those common in the wet spinning, because of the pre-formation of the filament and the previous evaporation of solvent.
  • the coagulation is more uniform due to the spontaneous establishment of a concentration gradient in the gas cylinder and coagulation bath and in the fiber itself;
  • the spinneret is not in a contact with the coagulation liquid, and therefore its corrosion is prevented.
  • the polymer is dissolved in a solvent mixture, it is preferred to establish the parameter to evaporate the most volatile solvent or an azeotropic mixture with minimum boiling point.
  • FIG. 2 The attachment for maintaining the interface between liquid and gas in the shaft at a constant chosen predefined elevation is seen in FIG. 2.
  • the space 6 between the spinneret and the surface level of the bath is evacuated by means of a vacuum pump not shown but indicated by the arrow A through the pipe 7.
  • the mouth 11 of the pipe is placed at the desired height of the level to be obtained and valve 12 is incorporated between the mouth 11 and the vacuum pump.
  • the valve comprises a seat 13 placed at its upper end in which a plug 14a formed at the end of float 14 is adapted to seat.
  • the float 14 is less dense than the coagulation liquid so that when the level in the shaft reaches the mouth 11, the valve 12 closes.
  • the valve 12 will open and the bath fills the vessel until it reaches to the mouth 11 again.
  • the conduit pipe 7 leads from the valve 12 to a separator device 15 into which the coagulation liquid flows.
  • the separator is equipped with three-way cock valve 16 at its bottom which is opened either towards a receiving vessel 17a or 17b. If either of the two vessels is full, the cock 16 is turned to the opposite position. Vacuum is eliminated in the full receiving vessel 17a or 17b by opening a cock valve 18:! or 18b, respectively, and the liquid is lead or discharged through the cock valve 19a or 19b back into the coagulation bath, at a rate to maintain the level in the system at the desired height.
  • Air, nitrogen, argon, carbon dioxide, etc. may be used as the gaseous medium flowing in space 6 below the spinneret.
  • the purpose of the circulation of the gas below the spinneret is to remove vapors of the solvent from this space to prevent saturation or the accumulation of an equilibrium concentration to be established there. Such saturation would prevent evaporation of the solvent from the filament stream.
  • FIG. 3 Apparatus for the circulation of the gaseous medium without influence of vacuum or pressure in the shaft is shown in FIG. 3.
  • the gas together with the desired amount of solvent vapor is sucked off through the outlet 9 by means of the pump 20.
  • the gas is cooled in the heat exchanger 21 where some part of the vapors condenses.
  • the condensed part of the solvent is separated from the gas in the separator 22 which is itself preferably cooled by a cooling jacket such as a Water or refrigerant system.
  • the gas is then led through the heater 23, the inlet 8 back into the space 6 between the spinneret 2 and the level of the bath 5.
  • the condensed solvent is let out of the separator 22 through three-way cock valve 16' alternately to the reservoirs 17'a and 17b.
  • the solvent may be recovered from the gaseous medium by condensation of the solvent vapors in a condenser, by absorption in a suitable liquid with a correspondingly high boiling point, or by adsorption on a solid surface (e.g. on charcoal).
  • a suitable liquid with a correspondingly high boiling point or by adsorption on a solid surface (e.g. on charcoal).
  • adsorption on a solid surface e.g. on charcoal
  • the outlet for sucking-off the solvent vapors is advantageously placed as near to the spinneret as possible, and it is particularly advantageous to place the outlet in the body of the spinneret, itself offset from the spinneret nozzle.
  • the method according to this invention is suitable for manufacturing all fibers spinnable from a solution.
  • it is more useful for spinning polymer solutions from which at least a part of solvents can be recovered by evaporation, as it is obvious from the previous description.
  • examples of such solutions are those of polyacrylonitrile in ethylene carbonate, dimethyl formamide, nitric acid or concentrated aqueous zinc chloride or sodium etc.
  • rhodanide solutions those of polyvinylchloride in cyclohexanone, those of chlorinated polyvinylchloride in acetone-alcohol mixtures, those of cellulose triacetate in methylene chloride, those of cellulose acetobutyrate in acetone, those of cellulose diacetate in acetone-alcohol mixtures. These examples should not be taken as limiting the use of the present invention.
  • the cylinder 4 in FIG. 1 may have any suitable crosssection, e.g. circular, squared, elliptical, etc. It may also be divided into two or more zones 25, 26, and 27 having different temperatures, and equipped with one or more heating or cooling jackets as seen in detail in FIG. 4. For instance, it is sometimes useful to keep different temperatures in adjacent portions of the spaces 6 in FIG. 4 and in the portion of the coagulation liquid in the cylinder 4. Also the temperatures of the coagulation liquid in the cylinder and in the coagulation bath need not be the same. It is especially advantageous, if the space between the spinneret and the level of the liquid zone 26 is heated, as well as the liquid, in the coagulation bath 5, while the liquid in the cylinder, zone 27, is cooled.
  • This measure helps to diminish the evaporation of the solvent from the surface of the coagulation liquid into the space 6 below the spinneret and, consequently, permits the rate of evaporation of the solvent from the jet stream of the polymer solution to rise. Moreover, it helps to enhance the conditions necessary for formation of a homogeneous fiber in the critical first stage (dry coagulation) of the coagulation. It also helps to equilibrate concentrations of the liquid in the shaft and in the coagulation bath by convection and maintains a uniform gradient. The elevated temperature of the coagulation bath is useful for accelerating the washing off of the solvent in the area, where the coagulation rate is no longer critical for the quality of the fiber.
  • a method of spinning a solution containing polymer dissolved in a solvent therefor, into fibrous filaments from a spinneret comprising the steps of extruding said polymer solutionfrom said spinneret, passing said extruded polymer solution through a field of gaseous medium held at subatmospheric pressure, into which a portion of said solvent is removed from said polymer solution, continuously supplying gaseous medium to said field and simultaneouly exhausting gaseous medium carrying said solvent therefrom and thereafter passing said remaining polymer solution into a liquid coagulating bath and coagulating said remaining solution to form filaments, said field of gaseous medium being maintained at a pressure less than that of said liquid coagulating bath and while at least part of the surface of said liquid coagulating bath is in direct contact with said field of gaseous medium, the level of that part of the surface of said coagulating bath being dependent on the pressure of said gaseous medium thereon.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Artificial Filaments (AREA)
US00316006A 1971-12-22 1972-12-18 Method for preparing fibers from polymer solutions Expired - Lifetime US3842151A (en)

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Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3996321A (en) * 1974-11-26 1976-12-07 E. I. Du Pont De Nemours And Company Level control of dry-jet wet spinning process
US4246221A (en) * 1979-03-02 1981-01-20 Akzona Incorporated Process for shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent
US4257999A (en) * 1977-08-10 1981-03-24 Bayer Aktiengesellschaft Process for the production of hydrophilic filaments and fibres by the dry jet wet-spinning method
US4261943A (en) * 1979-07-02 1981-04-14 Akzona Incorporated Process for surface treating cellulose products
US4386897A (en) * 1980-06-05 1983-06-07 Mobil Oil Corporation System for recovering film from pressurized extrusion zone
US4416698A (en) * 1977-07-26 1983-11-22 Akzona Incorporated Shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent and a process for making the article
US4484878A (en) * 1982-11-15 1984-11-27 Hermann Berstorff Maschinenbau Gmbh Filling level monitoring device
US4724109A (en) * 1983-12-28 1988-02-09 Denki Kagaku Kogyo Kabushiki Kaisha Process for production of continuous inorganic fibers and apparatus therefor
US4728473A (en) * 1983-02-28 1988-03-01 Asahi Kasei Kogyo Kabushiki Kaisha Process for preparation of polyparaphenylene terephthalamide fibers
US4820460A (en) * 1987-04-27 1989-04-11 Cuno, Incorporated Method of manufacturing a hollow porous fiber
US4883628A (en) * 1983-12-05 1989-11-28 Allied-Signal Inc. Method for preparing tenacity and modulus polyacrylonitrile fiber
US4915886A (en) * 1987-04-27 1990-04-10 Cuno, Incorporated Method of manufacturing nylon microporous hollow fiber membrane
WO1990006801A1 (en) * 1988-12-22 1990-06-28 Cuno, Incorporated Hollow fiber vertical quench bath
EP0526857A1 (en) * 1991-08-01 1993-02-10 Praxair Technology, Inc. Hollow fiber membranes
EP0750937A3 (en) * 1995-06-30 1997-10-15 Praxair Technology Inc Method and apparatus for spinning hollow fiber membranes
US20080220506A1 (en) * 2003-06-04 2008-09-11 University Of South Carolina Tissue scaffold having aligned fibrils, apparatus and method for producing the same, and artificial tissue and methods of use thereof
US20090160080A1 (en) * 2007-12-19 2009-06-25 Headinger Mark H High-speed meta-aramid fiber production
US20090160081A1 (en) * 2007-12-19 2009-06-25 Headinger Mark H Rapid plasticization of quenched yarns
US20090160079A1 (en) * 2007-12-19 2009-06-25 Headinger Mark H Single stage drawing for MPD-I yarn
US20090160082A1 (en) * 2007-12-19 2009-06-25 Headinger Mark H Multistage draw with relaxation step
WO2013050777A1 (en) 2011-10-06 2013-04-11 Nanoridge Materials, Incorporated Dry-jet wet spun carbon fibers and processes for making them using a nucleophilic filler/pan precursor
WO2013050779A1 (en) 2011-10-06 2013-04-11 Nanoridge Materials, Incorporated Formation of carbon nanotube-enhanced fibers and carbon nanotube-enhanced hybrid structures
CN105350091A (zh) * 2015-11-25 2016-02-24 山东大学 一种干喷湿纺喷丝装置及其制作方法
US10052807B2 (en) * 2014-02-12 2018-08-21 Fujifilm Corporation Fiber manufacturing method, non-woven fabric manufacturing method, and fiber manufacturing equipment

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04297746A (ja) * 1991-01-18 1992-10-21 Hitachi Air Conditioning & Refrig Co Ltd 空調装置
JP4910185B2 (ja) * 2004-07-30 2012-04-04 株式会社ヴァレオジャパン 異物除去装置を有する圧縮機

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB251680A (en) * 1925-01-30 1926-04-30 Leonard Angelo Levy Improvements in the production of artificial filaments
FR819146A (fr) * 1937-03-15 1937-10-11 Serrure pour machine à tricoter jacquard
US2581559A (en) * 1948-07-19 1952-01-08 Redding Mfg Company Inc Manufacture of filamentary articles

Cited By (32)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3996321A (en) * 1974-11-26 1976-12-07 E. I. Du Pont De Nemours And Company Level control of dry-jet wet spinning process
US4416698A (en) * 1977-07-26 1983-11-22 Akzona Incorporated Shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent and a process for making the article
US4257999A (en) * 1977-08-10 1981-03-24 Bayer Aktiengesellschaft Process for the production of hydrophilic filaments and fibres by the dry jet wet-spinning method
US4246221A (en) * 1979-03-02 1981-01-20 Akzona Incorporated Process for shaped cellulose article prepared from a solution containing cellulose dissolved in a tertiary amine N-oxide solvent
US4261943A (en) * 1979-07-02 1981-04-14 Akzona Incorporated Process for surface treating cellulose products
US4386897A (en) * 1980-06-05 1983-06-07 Mobil Oil Corporation System for recovering film from pressurized extrusion zone
US4484878A (en) * 1982-11-15 1984-11-27 Hermann Berstorff Maschinenbau Gmbh Filling level monitoring device
US4728473A (en) * 1983-02-28 1988-03-01 Asahi Kasei Kogyo Kabushiki Kaisha Process for preparation of polyparaphenylene terephthalamide fibers
US4883628A (en) * 1983-12-05 1989-11-28 Allied-Signal Inc. Method for preparing tenacity and modulus polyacrylonitrile fiber
US4724109A (en) * 1983-12-28 1988-02-09 Denki Kagaku Kogyo Kabushiki Kaisha Process for production of continuous inorganic fibers and apparatus therefor
US4820460A (en) * 1987-04-27 1989-04-11 Cuno, Incorporated Method of manufacturing a hollow porous fiber
US4915886A (en) * 1987-04-27 1990-04-10 Cuno, Incorporated Method of manufacturing nylon microporous hollow fiber membrane
WO1990006801A1 (en) * 1988-12-22 1990-06-28 Cuno, Incorporated Hollow fiber vertical quench bath
EP0526857A1 (en) * 1991-08-01 1993-02-10 Praxair Technology, Inc. Hollow fiber membranes
CN1034475C (zh) * 1991-08-01 1997-04-09 普拉塞尔技术有限公司 空心纤维膜
US5871680A (en) * 1995-06-30 1999-02-16 Praxair Technology, Inc. Method and apparatus for spinning hollow fiber membranes
EP0750937A3 (en) * 1995-06-30 1997-10-15 Praxair Technology Inc Method and apparatus for spinning hollow fiber membranes
US20080220506A1 (en) * 2003-06-04 2008-09-11 University Of South Carolina Tissue scaffold having aligned fibrils, apparatus and method for producing the same, and artificial tissue and methods of use thereof
US7878786B2 (en) * 2003-06-04 2011-02-01 University Of South Carolina Apparatus for producing tissue scaffold having aligned fibrils
US7771638B2 (en) * 2007-12-19 2010-08-10 E. I. Du Pont De Nemours And Company Rapid plasticization of quenched yarns
US20090160079A1 (en) * 2007-12-19 2009-06-25 Headinger Mark H Single stage drawing for MPD-I yarn
US20090160082A1 (en) * 2007-12-19 2009-06-25 Headinger Mark H Multistage draw with relaxation step
US7771637B2 (en) * 2007-12-19 2010-08-10 E. I. Du Pont De Nemours And Company High-speed meta-aramid fiber production
US7771636B2 (en) * 2007-12-19 2010-08-10 E. I. Du Pont De Nemours And Company Single stage drawing for MPD-I yarn
US20090160081A1 (en) * 2007-12-19 2009-06-25 Headinger Mark H Rapid plasticization of quenched yarns
US7780889B2 (en) * 2007-12-19 2010-08-24 E.I. Du Pont De Nemours And Company Multistage draw with relaxation step
US20090160080A1 (en) * 2007-12-19 2009-06-25 Headinger Mark H High-speed meta-aramid fiber production
WO2013050777A1 (en) 2011-10-06 2013-04-11 Nanoridge Materials, Incorporated Dry-jet wet spun carbon fibers and processes for making them using a nucleophilic filler/pan precursor
WO2013050779A1 (en) 2011-10-06 2013-04-11 Nanoridge Materials, Incorporated Formation of carbon nanotube-enhanced fibers and carbon nanotube-enhanced hybrid structures
US10052807B2 (en) * 2014-02-12 2018-08-21 Fujifilm Corporation Fiber manufacturing method, non-woven fabric manufacturing method, and fiber manufacturing equipment
CN105350091A (zh) * 2015-11-25 2016-02-24 山东大学 一种干喷湿纺喷丝装置及其制作方法
CN105350091B (zh) * 2015-11-25 2017-11-07 山东大学 一种干喷湿纺喷丝装置及其制作方法

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IT972745B (it) 1974-05-31
FR2164774A1 (enrdf_load_html_response) 1973-08-03
DD101923A5 (enrdf_load_html_response) 1973-11-20
GB1409530A (en) 1975-10-08
CH548459A (de) 1974-04-30
FR2164774B1 (enrdf_load_html_response) 1976-10-29
CA1025617A (en) 1978-02-07
DE2261996A1 (de) 1973-06-28
JPS4868809A (enrdf_load_html_response) 1973-09-19
CS160281B1 (enrdf_load_html_response) 1975-03-28

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