US3925525A - Spinning method - Google Patents

Spinning method Download PDF

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Publication number
US3925525A
US3925525A US387407A US38740773A US3925525A US 3925525 A US3925525 A US 3925525A US 387407 A US387407 A US 387407A US 38740773 A US38740773 A US 38740773A US 3925525 A US3925525 A US 3925525A
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Prior art keywords
spinning
passageway
range
equation
strain rate
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Expired - Lifetime
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US387407A
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Herman L Lanieve
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Celanese Corp
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Celanese Corp
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Priority to US387407A priority Critical patent/US3925525A/en
Priority to JP49090325A priority patent/JPS5076312A/ja
Priority to CA206,697A priority patent/CA1079015A/en
Priority to US05/594,010 priority patent/US4015924A/en
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Publication of US3925525A publication Critical patent/US3925525A/en
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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
    • D01D4/00—Spinnerette packs; Cleaning thereof
    • D01D4/02—Spinnerettes

Definitions

  • This invention relates to the spinning of synthetic filaments. More particularly, this invention relates to a novel method and apparatus for the spinning of synthetic filaments utilizing a spinneret nozzle designed to establish an essentially constant extensional strain rate.
  • spinnerets including a plurality of exit passageways in the form of nozzles or orifices machined in a spinneret plate.
  • a liquid comprising a polymer melt or a solution of a polymer in an appropriate solvent is extruded through these nozzles in the filament forming process.
  • the pressure drop across a spinneret can be expressed as the sum of the viscous dissipation in the passageway and the entrance and exit flows, the pressure due to kinetic energy effects, and that due to storage of elastic energy.
  • extrudate swell in connection with flow through a capillary is inversely related to the ratio of the capillary length to its diameter.
  • attempts to reduce extrudate swell by increasing that ratio may produce an excessive presure drop due to viscous dissipation.
  • the present invention departs from those prior art approaches to design of spinneret nozzle profiles which have been governed primarily by direct viscosity considerations, and perhaps, to some extent, inertial and turbulence considerations.
  • the present invention embodies a recognition that spinneret flow for fluids generally classified as viscous, such as PET melts or CTA solutions, is dominated by elastic" forces. More particularly, according to the present invention a nozzle profile is provided so as to establish an essentially constant extensional strain rate, viz. a constant change in veloc ity with respect to the incremental distance of fluid travel (an elastic force consideration). In this fashion the flow condition for the liquid is such as to provide for a low total pressure drop. At the same time adequate spinning speeds may be employed with acceptable die swell.
  • the essentially constant extensional strain rate leads to a low total pressure drop through several mechanisms.
  • a low constant extensional strain rate may be chosen to reduce that contribution as compared with prior art nozzle profiles.
  • the viscous pressure drop is minimized.
  • the gentle streamline entry flow provided by the nozzle profile of the present invention is believed to reduce dissipation due to vena contracta type eddies.
  • a preferred form of the invention intended to accomplish at least some of the foregoing objects entails the spinning of fibers through the provision of a spinneret plate for extruding polymeric materials and including at least one converging extrusion passageway having an entry opening and an exit orifice, with the passage profile being designed to establish an essentially constant extensional strain rate.
  • Spinning speeds in the range of about 500 to I500 meters per minute in the case of solution spinning and 500 to 6000 meters per minute in the case of melt spinning are usually appropriate, with about 1000 meters per minute and about 1200 to 3000 meters per minute being preferred respectively for dry and wet solution and for melt spinning.
  • Solution spinning temperatures of about 50 to l lC, preferably about 90C are usually contemplated.
  • temperatures in the range of about 275 to 330C, preferably 285 to 300C, are involved.
  • the approach angle defined as the angle of intersection between the axis of the converging extrusion passageway and the tangent to the wall of that passageway at the entrance opening, is between about to 45.
  • the passageway (i.e. the spinneret plate thickness) and exit orifice area may vary, with lengths in the range of about 0.020 to 0.060 inches for solution spinning and 0.1 to 0.6 inches for melt spinning, and areas in the range of about 3 X 10 to 50 X 10 square centimeters (solution spinning) and about l X l0 to 50 X 10 square centimeters (melt spinning) being desirable.
  • spinning of fiber-formin g materials by solution spinning (wet or dry) or melt spinning (without significant melt fracture in the range of operating conditions selected for the materials in contemplation for practice of the present invention) of any suitable polymeric materials, such as polyamides, polyesters, acrylics, polyimides, cellulosics, vinyl chloride and vinylidene cyanide polymerics and the like, may be practiced.
  • suitable polymeric materials such as polyamides, polyesters, acrylics, polyimides, cellulosics, vinyl chloride and vinylidene cyanide polymerics and the like.
  • Particular applicability of the present invention may be found in high speed spinning of cellulose esters or polyesters, especially polyethelene terephthalate.
  • the process is of particular value in the dry solution spinning of cellulose triacetate from solution in a solvent comprising a major amount of a halo genated hydrocarbon such as methylene chloride.
  • cellulose triacetate has reference to cellulose acetate having fewer than about 0.29 and preferably fewer than about 0.12 free hydroxyl group per anhydroglucose unit of the cellulose molecule, i.e., an ac etyl value calculated as combined acetic acid by weight of at least about 59 percent and preferably at least about 61 percent.
  • the dope solvent may comprise other halogenated lower alkanes such as ethylene dichloride or propylene chloride.
  • the dope solvent comprises a lower alkanol such as methanol, ethanol, isopropanol, etc.
  • the preferred dope solvent is methylene chloride-methanol in the proportions of about -10 by weight.
  • the cross-sectional configuration of the nozzle employed in accordance with the present invention is preferably symmetrical about the nozzle axis, with a circular cross-section being the preferred form.
  • non-circular configurations conventional in the spinning art such as for example those depicted in US. Pat. No. 3,303,530, issued Feb. 14, 1967, are also contemplated.
  • FIG. is a plan view of a spinneret in accordance with the present invention.
  • FIG. 2 is a sectional view taken along line 2-2 of FIG. 1;
  • FIG. 3 is an enlarged sectional view showing the profile of the exit passageway of the spinneret of FIGS. 1 and 2;
  • FIG. 4 is an enlarged sectional view showing the passageway of FIG. 3 contiguous, adjacent its entry end, with a frusto-conical passageway;
  • FIG. 5 is a schematic illustration of a dry spinning op eration in accordance with the present invention.
  • a spinneret or jet 10 in accordance with the present invention may be seen.
  • This spinneret is made of any suitable material such as stainless steel.
  • the spinneret is generally cupshaped.
  • the cup bottom indicated at 12 is provided with a plurality of circumferentially disposed, spaced apertures or exit passageways l4 therethrough.
  • a liquid comprising a polymer melt or a solution of a polymer in an appropriate solvent is supplied to the spinneret 10 and is extruded through the exit passageways I4 in the filament forming process.
  • An enlarged view of a preferred forms of the exit passageway 14 may be seen in FIGS. 3 and 4.
  • Each passageway 14 is in the form of a converging nozzle, the profile of which is hereinafter more fully described, that terminates in an exit orifice 16.
  • elastic energy stored in the liquid is recovered so as to result in extrudate swell or die swell. This storage of elastic energy occurs by reason of the extensional flow of the fluid.
  • FIG. 5 there is shown a dry spinning cabinet 20 to which dope is supplied through a pipe 22.
  • the liquid dope is extruded through the spinneret 10 of FIGS. l-3 with no intervening plating of the spinneret.
  • I-Iot air may be admitted to the cabinet 20 through a suitable conduit 23 and may be exhausted through a suitable conduit 24 along with vapors of the dope solvent.
  • the filaments 26 leaving the spinneret 10 through the extrusion passageways 14 are directed about a guide 28 and out of the cabinet at a location indicated at 30.
  • the filaments are pulled as a yarn 32 by suitable draw rolls 34.
  • the yarn 32 by suitable draw rolls 34.
  • the yarn 32 passes through a guide 36 and is twisted and taken up on a bobbin 38 by a conventional collector such as a ring spinner 40.
  • the nozzle profile in accordance with the present invention may be more fully appreciated.
  • the radius of the exit ori- 1 fice 16 is indicated by R.
  • the nozzle preferably is circular in transverse cross-section, and has smooth, gradually curving walls 18 in the form of a surface of revolution defined by a generatrix moving about the central axis 19 of the passageway 14.
  • the wall profile, conforming to the shape of this generatrix, provides an essentially constant extensional strain rate during flow of the polymeric material through the passageway 14 by being designed to essentially respond to the following cubic equation:
  • R is the radius of the exit orifice l6
  • r u is the wall radius measured perpendicular to the axis 22;
  • Z is the distance along the axis 19 of the nozzle measured from the exit orifice 16;
  • A is a constant hereinafter more fully described.
  • Equation (1) may be derived by integrating the following equation:
  • 6v/6Z is the extensional strain rate represented by the partial derivative of velocity (V) with respect to distance measured from the exit orifice 16 along the nozzle axis 19;
  • V is the fluid velocity
  • Q is the volumetric flow rate. and while also recalling the limit condition that )1! is equal to R [as defined for equation (l)]at the exit orifree 16.
  • the constant A of Equation (l) is determined by equating the constant extensional strain rate K of Equation (2) with the maximum extensional strain rate for a conical spinneret wherein the die swell is acceptable (hereinafter referred to as equivalent conical spinneret"). Then,
  • Sv/SZ max. cone is the maximum extensional strain 55 rate for the equivalent conical spinneret.
  • the well known equation for the wall profile of a conical spinneret is:
  • Equation l rm and Z are as defined in Equation l); and 6 is the half angle of the equivalent conical spinneret,
  • Equations (2) through (6) may then be combined and integrated to produce equation (1) where A of equation (l) will be defined as:
  • Equation (8) and (9) yields:
  • Equation (ll) is rearranged and substituted in Equation (10), it will be seen that Since 5v/8Z appears in the denominator of Equation (l2), the largest possible value of 8v/5Z provides the smallest viscous pressure drop (APv) However, the provision for a constant extensional strain rate inherently imposes the constraint that:
  • FIG. 4 a further nozzle passageway that may be employed according to the present invention may be seen.
  • the passageway of FIG. 4 is comprised of the nozzle passage 14 of FIG. 3 contiguous with a passageway extension 42 in the form of a frusto-conical countersink. It has been found that manufacturing of the spinneret with a passageway 14 profile establishing an essentially constant extensional strain rate as discussed above is more convenient when such a countersink is provided.
  • the intersection of the conical section 42 with the passageway 14 be such that the walls of the cone are tangent to the walls 18 of the passageway 14 at its entry orifice 17. If such tangency is not provided, and the cone makes a steeper angle than the tangent then the extensional strain rate in the conical section 42 will be greater. As such, the chosen die-swell characteristics will not be met, and viscous pressure drop will be greater than the minimum which the constant extensional strain rate otherwise would provide.
  • r w is the perpendicular distance between nozzle wall and points along that axis
  • Z is the distance along that axis measured from said exit orifice
  • A is a constant.
  • said protile is defined by a surface of revolution defined by a generatrix described by said equation and moving about said axis in a generally circular path.
  • a solution spinning method according to claim 3 wherein said liquid material consists essentially of cellulose acetate and wherein said material is extruded at spinning speeds in the range of about 500 to 1500 meters per minute at spinning temperatures of about 50 to ll0C.
  • a melt spinning method according to claim 3 wherein said liquid material consists essentially of polyethylene terephthalate and wherein said material is extruded at spinning speeds in the range 500 to 6000 meters per minute at spinning temperatures of about 275 to 330C.
  • liquid material comprises polyethylene terephthalate.
  • a solution spinning method according to claim I wherein said material is extruded at spinning speeds in the range of about 500 to 1500 meters per minute.
  • a melt spinning method according to claim 1 wherein said material is extruded at spinning speeds in the range of about 500 to 3000 meters per minute.
  • equation (7) should read:

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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)
US387407A 1973-08-10 1973-08-10 Spinning method Expired - Lifetime US3925525A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US387407A US3925525A (en) 1973-08-10 1973-08-10 Spinning method
JP49090325A JPS5076312A (enrdf_load_stackoverflow) 1973-08-10 1974-08-08
CA206,697A CA1079015A (en) 1973-08-10 1974-08-09 Spinning method and apparatus
US05/594,010 US4015924A (en) 1973-08-10 1975-07-08 Spinning apparatus providing for essentially constant extensional strain rate

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US387407A US3925525A (en) 1973-08-10 1973-08-10 Spinning method

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US05/594,010 Division US4015924A (en) 1973-08-10 1975-07-08 Spinning apparatus providing for essentially constant extensional strain rate

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JP (1) JPS5076312A (enrdf_load_stackoverflow)
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Cited By (51)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4384098A (en) * 1981-01-13 1983-05-17 Phillips Petroleum Company Filamentary polypropylene and method of making
US5234652A (en) * 1990-12-20 1993-08-10 Woodhams Raymond T Process for the continuous production of high modulus articles from high molecular weight plastics
US5236734A (en) * 1987-04-20 1993-08-17 Fuisz Technologies Ltd. Method of preparing a proteinaceous food product containing a melt spun oleaginous matrix
US5238696A (en) * 1987-04-20 1993-08-24 Fuisz Technologies Ltd. Method of preparing a frozen comestible
US5240665A (en) * 1991-12-31 1993-08-31 Eastman Kodak Company Process of making cellulose acetate fibers from spinning solutions containing metal oxide precursor
US5268110A (en) * 1991-05-17 1993-12-07 Fuisz Technologies Ltd. Oil removing method
US5279849A (en) * 1992-05-12 1994-01-18 Fuisz Technologies Ltd. Dispersible polydextrose, compositions containing same and method for the preparation thereof
US5286513A (en) * 1987-04-20 1994-02-15 Fuisz Technologies Ltd. Proteinaceous food product containing a melt spun oleaginous matrix
WO1994012703A1 (en) * 1992-12-03 1994-06-09 The Dow Chemical Company Method for spinning a polybenzazole fiber
US5330348A (en) * 1992-08-05 1994-07-19 E. I. Du Pont De Nemours And Company Spinneret for the production of hollow filaments
US5346377A (en) * 1993-10-07 1994-09-13 Fuisz Technologies Ltd. Apparatus for flash flow processing having feed rate control
US5348758A (en) * 1992-10-20 1994-09-20 Fuisz Technologies Ltd. Controlled melting point matrix formed with admixtures of a shearform matrix material and an oleaginous material
US5380473A (en) * 1992-10-23 1995-01-10 Fuisz Technologies Ltd. Process for making shearform matrix
US5387431A (en) * 1991-10-25 1995-02-07 Fuisz Technologies Ltd. Saccharide-based matrix
US5407676A (en) * 1990-12-14 1995-04-18 Fuisz Technologies Ltd. Hydrophilic form of perfluoro compounds and a method of manufacture
US5427804A (en) * 1992-03-05 1995-06-27 Fuisz Technologies Ltd. Low-fat edible proteins with maltodextrins and low-saturate oils
US5445769A (en) * 1994-06-27 1995-08-29 Fuisz Technologies Ltd. Spinner head for flash flow processing
US5456932A (en) * 1987-04-20 1995-10-10 Fuisz Technologies Ltd. Method of converting a feedstock to a shearform product and product thereof
US5458823A (en) * 1994-10-28 1995-10-17 Fuisz Technologies Ltd. Method and apparatus for spinning feedstock material
US5472731A (en) * 1987-04-20 1995-12-05 Fuisz Technologies Ltd. Protein based food product
US5501858A (en) * 1992-05-12 1996-03-26 Fuisz Technologies Ltd. Rapidly dispersable compositions containing polydextrose
US5516537A (en) * 1987-04-20 1996-05-14 Fuisz Technologies Ltd. Frozen comestibles
US5518730A (en) * 1992-06-03 1996-05-21 Fuisz Technologies Ltd. Biodegradable controlled release flash flow melt-spun delivery system
US5518551A (en) * 1993-09-10 1996-05-21 Fuisz Technologies Ltd. Spheroidal crystal sugar and method of making
US5549917A (en) * 1994-07-01 1996-08-27 Fuisz Technologies Ltd. Flash flow formed solloid delivery systems
US5556652A (en) * 1994-08-05 1996-09-17 Fuisz Technologies Ltd. Comestibles containing stabilized highly odorous flavor component delivery systems
US5567439A (en) * 1994-06-14 1996-10-22 Fuisz Technologies Ltd. Delivery of controlled-release systems(s)
US5576042A (en) * 1991-10-25 1996-11-19 Fuisz Technologies Ltd. High intensity particulate polysaccharide based liquids
US5587198A (en) * 1995-05-31 1996-12-24 Fuisz Technologies Ltd. Positive hydration method of preparing confectionery and product therefrom
US5593502A (en) * 1993-10-07 1997-01-14 Fuisz Technologies Ltd. Method of making crystalline sugar and products resulting therefrom
US5622719A (en) * 1993-09-10 1997-04-22 Fuisz Technologies Ltd. Process and apparatus for making rapidly dissolving dosage units and product therefrom
US5624684A (en) * 1991-05-17 1997-04-29 Fuisz Technologies Ltd. Enzyme systems
US5651987A (en) * 1991-12-17 1997-07-29 Fuisz Technologies Ltd. Ulcer prevention and treatment composition
US5654003A (en) * 1992-03-05 1997-08-05 Fuisz Technologies Ltd. Process and apparatus for making tablets and tablets made therefrom
US5728397A (en) * 1992-05-12 1998-03-17 Fuisz Technologies Ltd. Polydextrose product and process
US5779946A (en) * 1993-04-19 1998-07-14 Fuisz Technologies Ltd. Method for spin processing material having temperature feedback control
US5843922A (en) * 1994-07-29 1998-12-01 Fuisz Technologies Ltd. Preparation of oligosaccharides and products therefrom
US5851553A (en) * 1993-09-10 1998-12-22 Fuisz Technologies, Ltd. Process and apparatus for making rapidly dissolving dosage units and product therefrom
US5895664A (en) * 1993-09-10 1999-04-20 Fuisz Technologies Ltd. Process for forming quickly dispersing comestible unit and product therefrom
US6020002A (en) * 1994-06-14 2000-02-01 Fuisz Technologies Ltd. Delivery of controlled-release system(s)
US6051175A (en) * 1993-09-03 2000-04-18 Polymer Processing Research Inst., Ltd. Process for producing filament and filament assembly composed of thermotropic liquid crystal polymer
WO2001089023A1 (en) * 2000-05-19 2001-11-22 Korea Institute Of Science And Technology A lithium secondary battery comprising a super fine fibrous polymer electrolyte and its fabrication method
WO2001089021A1 (en) * 2000-05-19 2001-11-22 Korea Institute Of Science And Technology A composite polymer electrolyte, a lithium secondary battery comprising the composite polymer electrolyte and their fabrication methods
WO2001089022A1 (en) * 2000-05-19 2001-11-22 Korea Institute Of Science And Technology A lithium secondary battery comprising a super fine fibrous polymer separator film and its fabrication method
WO2001089020A1 (en) * 2000-05-19 2001-11-22 Korea Institute Of Science And Technology A hybrid polymer electrolyte, a lithium secondary battery comprising the hybrid polymer electrolyte and their fabrication methods
WO2001091222A1 (en) * 2000-05-22 2001-11-29 Korea Institute Of Science And Technology A lithium secondary battery comprising a polymer electrolyte fabricated by a spray method and its fabrication method
WO2001091219A1 (en) * 2000-05-22 2001-11-29 Korea Institute Of Science And Technology A lithium secondary battery comprising a porous polymer separator film fabricated by a spray method and its fabrication method
WO2001091221A1 (en) * 2000-05-22 2001-11-29 Korea Institute Of Science And Technology A composite polymer electrolyte fabricated by a spray method, a lithium secondary battery comprising the composite polymer electrolyte and their fabrication methods
WO2001091220A1 (en) * 2000-05-22 2001-11-29 Korea Institute Of Science And Technology A hybrid polymer electrolyte fabricated by a spray method, a lithium secondary battery comprising the hybrid polymer electrolyte and their fabrication methods
US20050258562A1 (en) * 2004-05-21 2005-11-24 3M Innovative Properties Company Lubricated flow fiber extrusion
US20130183525A1 (en) * 2012-01-12 2013-07-18 Beijing University Of Chemical Technology Methods of Preparing Polyimide Fibers with Kidney-Shaped Cross-Sections

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JPS5567007A (en) * 1978-11-10 1980-05-20 Unitika Ltd Production of ultra-fine polyamide fiber
JPS61138719A (ja) * 1984-12-10 1986-06-26 Sumitomo Chem Co Ltd 溶融紡糸方法
JP2668849B2 (ja) * 1993-12-02 1997-10-27 惠一 村上 紡糸用口金の製造方法
US6682677B2 (en) * 2000-11-03 2004-01-27 Honeywell International Inc. Spinning, processing, and applications of carbon nanotube filaments, ribbons, and yarns
JP2017179622A (ja) * 2016-03-28 2017-10-05 帝人株式会社 コポリパラフェニレン・３，４’−オキシジフェニレンテレフタルアミド繊維の製造方法

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US2742667A (en) * 1951-11-08 1956-04-24 Rhodiaceta Spinnerets
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Cited By (79)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4384098A (en) * 1981-01-13 1983-05-17 Phillips Petroleum Company Filamentary polypropylene and method of making
US5374447A (en) * 1987-04-20 1994-12-20 Fuisz Technologies Ltd. Method of preparing a reduced-fat meat product
US5286513A (en) * 1987-04-20 1994-02-15 Fuisz Technologies Ltd. Proteinaceous food product containing a melt spun oleaginous matrix
US5238696A (en) * 1987-04-20 1993-08-24 Fuisz Technologies Ltd. Method of preparing a frozen comestible
US5490993A (en) * 1987-04-20 1996-02-13 Fuisz Technologies Ltd. Method of preparing a proteinaceous food product containing a melt spun matrix and product thereof
US5472731A (en) * 1987-04-20 1995-12-05 Fuisz Technologies Ltd. Protein based food product
US5516537A (en) * 1987-04-20 1996-05-14 Fuisz Technologies Ltd. Frozen comestibles
US5503862A (en) * 1987-04-20 1996-04-02 Fuisz Technologies Ltd. Method of subjecting a protein-containing material to flash flow processing and product thereof
US5456932A (en) * 1987-04-20 1995-10-10 Fuisz Technologies Ltd. Method of converting a feedstock to a shearform product and product thereof
US5236734A (en) * 1987-04-20 1993-08-17 Fuisz Technologies Ltd. Method of preparing a proteinaceous food product containing a melt spun oleaginous matrix
US5407676A (en) * 1990-12-14 1995-04-18 Fuisz Technologies Ltd. Hydrophilic form of perfluoro compounds and a method of manufacture
US5234652A (en) * 1990-12-20 1993-08-10 Woodhams Raymond T Process for the continuous production of high modulus articles from high molecular weight plastics
US5399308A (en) * 1990-12-20 1995-03-21 Woodhams; Raymond T. Process for the continuous production of high modulus articles from high molecular weight plastics
US5624684A (en) * 1991-05-17 1997-04-29 Fuisz Technologies Ltd. Enzyme systems
US5268110A (en) * 1991-05-17 1993-12-07 Fuisz Technologies Ltd. Oil removing method
US6129926A (en) * 1991-05-17 2000-10-10 Fuisz Technologies Ltd. Flash flow processing of thermoplastic polymers and products made therefrom
US5709876A (en) * 1991-10-25 1998-01-20 Fuisz Technologies Ltd. Saccharide-based matrix
US5429836A (en) * 1991-10-25 1995-07-04 Fuisz Technologies Ltd. Saccharide-based matrix
US5387431A (en) * 1991-10-25 1995-02-07 Fuisz Technologies Ltd. Saccharide-based matrix
US5576042A (en) * 1991-10-25 1996-11-19 Fuisz Technologies Ltd. High intensity particulate polysaccharide based liquids
US5597608A (en) * 1991-10-25 1997-01-28 Fuisz Technologies Ltd. Saccharide-based matrix incorporating maltodextrin and process for making
US5651987A (en) * 1991-12-17 1997-07-29 Fuisz Technologies Ltd. Ulcer prevention and treatment composition
US5240665A (en) * 1991-12-31 1993-08-31 Eastman Kodak Company Process of making cellulose acetate fibers from spinning solutions containing metal oxide precursor
US5654003A (en) * 1992-03-05 1997-08-05 Fuisz Technologies Ltd. Process and apparatus for making tablets and tablets made therefrom
US5427804A (en) * 1992-03-05 1995-06-27 Fuisz Technologies Ltd. Low-fat edible proteins with maltodextrins and low-saturate oils
US5501858A (en) * 1992-05-12 1996-03-26 Fuisz Technologies Ltd. Rapidly dispersable compositions containing polydextrose
US5728397A (en) * 1992-05-12 1998-03-17 Fuisz Technologies Ltd. Polydextrose product and process
US5279849A (en) * 1992-05-12 1994-01-18 Fuisz Technologies Ltd. Dispersible polydextrose, compositions containing same and method for the preparation thereof
US5518730A (en) * 1992-06-03 1996-05-21 Fuisz Technologies Ltd. Biodegradable controlled release flash flow melt-spun delivery system
US5330348A (en) * 1992-08-05 1994-07-19 E. I. Du Pont De Nemours And Company Spinneret for the production of hollow filaments
US5348758A (en) * 1992-10-20 1994-09-20 Fuisz Technologies Ltd. Controlled melting point matrix formed with admixtures of a shearform matrix material and an oleaginous material
US5380473A (en) * 1992-10-23 1995-01-10 Fuisz Technologies Ltd. Process for making shearform matrix
WO1994012703A1 (en) * 1992-12-03 1994-06-09 The Dow Chemical Company Method for spinning a polybenzazole fiber
US5779946A (en) * 1993-04-19 1998-07-14 Fuisz Technologies Ltd. Method for spin processing material having temperature feedback control
US6051175A (en) * 1993-09-03 2000-04-18 Polymer Processing Research Inst., Ltd. Process for producing filament and filament assembly composed of thermotropic liquid crystal polymer
US5601076A (en) * 1993-09-10 1997-02-11 Fuisz Technologies Ltd. Spheroidal crystal sugar and method of making
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