US3361859A - Melt-spinning process - Google Patents

Melt-spinning process Download PDF

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US3361859A
US3361859A US554620A US55462066A US3361859A US 3361859 A US3361859 A US 3361859A US 554620 A US554620 A US 554620A US 55462066 A US55462066 A US 55462066A US 3361859 A US3361859 A US 3361859A
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filaments
spinning
melt
temperature
polymer
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Cenzato Lorenzo
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EIDP Inc
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EI Du Pont de Nemours and Co
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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
    • D01D5/08—Melt spinning methods
    • D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
    • 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
    • D01D5/08—Melt spinning methods
    • D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes

Definitions

  • This invention is concerned with the preparation of filaments from high melting, highly viscous polymers by melt spinning, cooling to solidify the filaments and then drawing the filaments.
  • the present invention is an improvement in the process of extruding synthetic organic polymer through spinneret orifices at atemperature (T at least 20 C. above the melting point (T of the polymer, cooling the extruded polymer in a gaseous medium to form filaments, and thereafter drawing the filaments at least 2.8x to a tenacity of at least 4 grams per denier (g.p.d.).
  • the improvement is in providing a controlled retarded cooling of the filaments by heating the gaseous medium to have gas temperatures (T adjacent to the filaments which are less than T +100 C.
  • melt 17 melt 6200 The improvement is particularly applicable to the meltspinning of polymers such as polyethylene terephthalate under conditions such that 1; melt times the spinning speed (V) in yards per minute is greater than 15 10 poisesy.p.rn.
  • the process is particularly useful in the preparation of fibers of high viscosity polymer for industrial purposes where tenacities of 8 g.p.d. or more are needed.
  • a high viscosity polyester (1 melt of 6200 or more) is preferably extruded at temperatures of 320 C. or more into hot gas having a temperature of at least 320 C.
  • the extruded fiber is solidi- T ++50 log r3 fied under the retarded cooling conditions specified, and the cooled fibers are drawn at least 6X.
  • the gas temperatures (T are less than T mi I 6200 s n 7 melt and preferably the maximum temperature of the hot gas (T is at least T 20 C. adjacent to the spinneret.
  • the temperature of the gas (T should be controlled critically until it reaches a value of (T -60) after which it can cool very quickly. This is equivalent to a T T value of about 120 C. for the examples of polyesters given subsequently.
  • Normally AT will occur adjacent to the spinneret. However, it may be delayed for as much as 0.12 to 0.15 seconds with some types of heating and particularly with negative AT values, as when T increases from an initial value to a maximum and is then cooled.
  • the process of this invention is particularly valuable in processes where spinning orifices of 6 to 30 mils in diameter are used with spin stretch ratios [(Orifice DiameterV/(as-spun fiber diameter) of up to 100 to produce as-sp-un fibers of 6 to 200 d.p.f. for drawing at draw ratios of 3.5 or more.
  • inert gas i.e., a gas substantially free of oxygen.
  • Suitable inert gases are hot nitrogen and carbon dioxide, as well as inert organic vapors.
  • the use of an oxygen-free gas immediately below the spinneret reduces degradation encountered at that point when polymers, such as poly(ethylene terephthalate) having a relative viscosity (RV) above about 50 or 55, are extruded into air.
  • the use of an oxygen-free gas can reduce the normally encountered relative viscosity loss by as much as 5 to 6 units, while at the same time reducing the normally encountered gain in carboxyl group content by as much as 6 to 8 eq./10 g.
  • the improvement obtained with an inert gas is even more pronounced when higher RV polymers are used, i.e., 75-100.
  • Threadline tension Polymer RV (grams/denier) Maximum Preferred Both the spinning speed and the threadline tension refer to measurements made after the filaments have cooled below the second-order transition temperature and before being subjected to increased tension in any subsequent drawing operation which may be coupled with the spinning process.
  • the spinning speed is preferably less than 1300 yards per minute and, in a coupled spinning and drawing process, should preferably be about 200 to 500 yards .per minute (the wind-up speed after drawing in a coupled process is muchhigher, of course).
  • the products made :by the improved process of the present invention are characterized by an improved uniformity of structure within the shaped articles and between simultaneously extruded articles.
  • the products made by extrusion alone are noted for their lower levels of birefringence and lack of orientation when compared to products made at the same speeds using conventional processes.
  • fibers made by the present invention have a greatly reduced gradient across the fiber crosssection.
  • the oriented filaments of this invention also show an improved intrafilament uniformity over known products.
  • the improvement in polyester filaments is especially pronounced, as illustrated in the drawings wherein FIGURE 1 is an electron micrograph (26,000Xmagnification) of a typical filament of this invention.
  • FIGURE 2 is a corresponding micrograph of a filament which is typical of the prior art.
  • Polyester filaments of the prior art contain a skin of about /2 micron thick that can be peeled from the fiber. This skin shows the first arc. (003 Miller Index) on the axis corresponding to the fiber axis in an electron diffraction pattern to be indistinct and single. A diffraction pattern of the whole fiber shows the same are as sharp and split into two maxima. Boththe peeling and the whole fiber of products of this invention show the first are on the axis as sharp and split into two maxima, thus showing the uniformity. of the new product.
  • the oriented products of this invention also display a very high level of crystallinity in conjunction with excellent physical properties such as lack of brittleness, high 140 C. flex resistance, high tenacity and excellent resistance to fibrillation which has not been previously attained.
  • Polyethylene terephthalate fibers with a denier per filament greater than 2.5 and having a flex life of considerably more than 200,000 cycles at 140 C. are obtained.
  • the improved interfilament uniformity of the oriented filaments of this invention is shown by such properties as a ratio of yarn to average single filament tenacity of 0.9 or greater and by the substantially straight and sharp stress-strain curves obtained on yarn.
  • the invention provides improved results with polypropylene, and the new higher melting, higher density forms of polypropylene having a decreased amount of chain branching and/or isotactic structures are particularly suitable in this process.
  • the condensation polymers and copolymers e.g., polyamides and polyesters, and particularly those that can be readily melt polymerized to high viscosity, are preferred for application in this method.
  • Suitable polymers include fiber-forrning polyamides and polyesters of types described, e.g., in U.S. Patents Nos.
  • Particularly suitable polyamides include polyhexamethylene adiparnide and polyamides of alkanedioic acids with diaminohydrocarbons [preferably bis (para-aminocyclohexyl)methane], where the hydrocarbon portion is a divalent, saturated, cycloaliphatic group.
  • the preferred polyesters to be used in this invention are obtained from terephthalic acid wherein at least 75% of the recurring structural units of the polyester are glycol terephthalate structural units. These should be fiberfonning and have a relative viscosity of at least about 25.
  • Such polymers may be represented in a more general way by the formula HOG(OOCA-COOG),YOH where G and A- are divalent organic radicals corresponding, respectively, to the radical in the initial glycol, G(OH) and to the initial dicarboxylic acid, A(COOH) and y is a number sufiicient that the polymer is of fiber-forming molecular weight; at least about 75% of the A- radicals being terephthalate radicals.
  • the terephthalate radical may be the sole dicarboxylate constituent of the recurring structural units, or up to about 25% of the recurring structural units may contain other dicarboxylic radicals, such as the adipate, sebacate, isophthalate, S-(sodium sulfo)-isophthalate, bibenzoate, hexahydroterephthalate, diphenoxyethane-4,4'-dicarboxylate, or p,p'-sulfonylbibenzoate radicals, derived from the corresponding dicarboxylic acids or ester-forming derivatives thereof.
  • dicarboxylic radicals such as the adipate, sebacate, isophthalate, S-(sodium sulfo)-isophthalate, bibenzoate, hexahydroterephthalate, diphenoxyethane-4,4'-dicarboxylate, or p,p'-sulfonylbibenzoate radicals, derived
  • the glycol may be trimethylene glycol, tetramethylene glycol, hexamethylene glycol, decamethylene glycol, 2,2-dimethylpropanediol, trans-p-hexahydroxylylene glycol, diethylene glycol, bis-p-(fi-hydroxyethoxy) benzene, bis-1,4-(l3-hydroxyethoxy) -2,5-dichlorobenzene, or his [p (,8 hydroxyethoxy)phenyl]difiuoromethane.
  • Those may be used alone or in mixtures, e.g., ethylene glycol plus up to about 25 mol percent of the abovementioned glycols.
  • the flex life (flex resistance) of a filament is determined by clamping one end of a filament of at least one inch length to a frame rotating in the plane of the vertical with the filament being weighted by an amount of 0.6 gram per denier (g.p.d.) and having a smooth wire 3 mils in diameter positioned horizontally at the midpoint of the filament. Twenty-one specimens are simultaneously bent repeatedly through over the Wire while under tension. The number of cycles required to cause failure of 11 filaments is accepted as the test result.
  • the relative viscosity is the viscosity of a solution of polymer relative to that of the solvent and is a measure or" the molecular weight.
  • the polyamide solutions contain 5.5 g. of polymer in 50 ml. of formic acid or of formic acid/phenol (50/50 by weight), and the viscosity is measured at 25 C.
  • the polyester solutions contain 2.15 parts of the polymer in 19.35 parts by weight of a 7/10 mixture of 2,4,6-trichlorophenol/phenol and the viscosity is measured at 25 C.
  • T Gas temperatures (T should be measured with an aspirating thermocouple placed as close as possible to the filaments without disrupting the spinning. The hot gas is drawn in over a thermocouple that is shielded from radiation of the equipment.
  • the maximum draw ratio of a fiber is determined by drawing (or stretching) a fiber around a metal pin, over a plate, or through a bath at a given temperature by means of a feed and a delivery roll having continuously variable speeds to the maximum amount possible without breaking the fibers.
  • Draw ratio is defined as the ratio of the surface speeds of the delivery roll to the feed roll or the ratio of the drawn length to the as-spun length of the fiber. Unless otherwise noted, all physical properties are determined on fibers drawn to the maximum draw ratio.
  • Example I Poly(ethylene terephthalate) of relative viscosity 40.5 (crystalline melting point of 265 C.) and containing 0.15% TiO is extruded from a melt at 288" C. through a spinneret containing 20 holes of 16 mils in diameter located on a 2%" diameter circle at 285 C. and the filament (23 d.p.f.) wound up at 500 y.p.m. Cooling of the filaments is retarded under controlled temperature conditions with a muffle furnace (7" high), comprising exposed electrical resistance wires coiled on the inner surface of a ceramic cylinder affording an open passageway of about 3" in diameter, centered below the spinneret.
  • the apparatus may be arranged as disclosed in Hardy U.S. Patent No.
  • thermocouples are carefully inserted between two adjacent filaments at the uper and lower edge of the furnace so that they measure the temperature of the air between each pair of filaments.
  • a third thermocouple is located half Way up the muflle furnace approximately of an inch towards the threadline from the heating element.
  • Item 01 represents the values on filaments spun from the same polymer at the same speed and spinneret temperature but using conventional cross flow cooling as disclosed in US. Patent No. 2,273,105.
  • the improvement in properties of the filaments spun under the process of this invention is apparent from the data.
  • the temperatures indicated for items a, b and 0 fall within the previously defined limits of AT.
  • polyester poly(trans-p-hexahydroxylene terephthalate) of relative viscosity 39
  • copolyester poly[ethyleneterephthalate/S-(sodium-sulfo)isophthalate] 98/2 mol percent ratio, of relative viscosity 18.5, are separately spun under conditions within the above limits.
  • Example II This example shows additional unexpected properties of the polyester filaments of this invention.
  • a control yarn is prepared from poly(ethylene terephthalate) of 45 relative viscosity, i.e., of higher molecular weight than the above polymer.
  • the yarn is prepared under the best possible conventional quench spinping conditions, using a cross-flow quench and advancing the solidified filaments at 150 y.p.m. to a drawing step as above for maximum drawability.
  • higher molecular weight of the polymer used when processed in accordance with the present invention, higher molecular weight polymer normally provides improved tenacity and flex resistance
  • the single filaments have a tenacity of only 7.5 g.p.d. and the yarn has a tenacity of only 6.5 g.p.d. (86% of filament value).
  • Product A has a significantly higher degree of crystallinity than the control (a crystallinity index number of 39 vs. 36 for the control-ASTM International Symposium, October, 1958, by W. Stratton).
  • the actual level of crystallinity depends upon the heat treatment of the fiber or film. It has been observed that under the same heating conditions the products of this invention give a higher level of crystallinity than products spun under conventional methods.
  • the flex life of product A is 560,000 cycles compared to 86,000 cycles for the control when tested as described previously at 140 C.
  • the tenacity of the filaments not broken by the flexing is 8.9 g.p.d. as contrasted with 4.8 g.p.d. for the control.
  • Photomicrographs of the ends of the filaments broken in the test show filaments A to have a clean break'with no signs of fibrillation (i.e., splitting Whereas the control ends are completely frayed and fibrillated.
  • FIGURES 1 and 2 Electron micrographs (26,000 times magnification) of the replicas of product A and the control are shown in FIGURES 1 and 2 respectively.
  • the upper dark portions represent the surface of the fiber
  • the light central area represents a skin of about 1.5 micron in thickness
  • the darker area at the bottom represents one-half of the core of the filament.
  • the transversal structural uniformity of fiber A is apparent in FIGURE 1.
  • the skin and core can scarcely be distinguished, both exhibiting high crystallinity and orientation.
  • the skin of the control (FIG. 2) exhibits low crystallinity and orientation, and is markedly different from the core.
  • a second control yarn is prepared of the same polymer but spun at 600 y.p.m. under optimum quench-spinning conditions. It has a maximum filament tenacity of 5.9 g.p.d., a maximum yarn tenacity of 5.1 g.p.d. (87% of filament tenacity) and a flex life of les than 100,000 cycles at 140 C.
  • Example Ill Yarns are prepared according to the conditions of items (b) and (d) (control) in Example I, but drawn 5.2 and 4.7 times (maximum possible) over a C. hot pin.
  • the physical properties of the drawn yarn are shown below:
  • the heater used in this example comprises two concentric aluminum tubes 11 inches long.
  • the inner tube through which the filaments pass has an inside diameter of 8 inches.
  • Resistance heaters are located in the annulus between the 2 tubes and are controlled by a thermocouple adjacent to the wall of the central passage and located about 2 inches below the top.
  • the heater annulus has a metal bottom which, along with the outside face of the heater, is well insulated.
  • the heater is mounted to the spinning head through a 1-inch layer of hard insulating material so that the heater and insulation provides a chamber, open to air only at the bottom that extends 12 inches down from the face of the spinneret.
  • Molten poly(ethylene terephthalate) is extruded through a spinneret having 192 holes of 0.3 mm. diameter.
  • the extruded filaments pass through the heater and are then gently quenched by a conventional cross-flow of air from one side of the threadline, Birefringence is determined on samples of the asspun (undrawn) filaments.
  • Item 5 shows the effect of a low spinning velocity (200 y.p.m.) as compared to item 4 at 350 y.p.m. using the same heater control temperature and having the same maximum T Items 6 and 3 can also be compared for different speeds at the same heater temperature and similar maximum T values. The necessity for cooling the fibers more slowly at the higher speed is apparent from the birefringence values in Table 3.
  • Item 7 is prepared as above but with the addition of a 4 inch insulated tube to the bottom of the heater. This decreases the rate of cooling over that afi'orded by the heater alone. When the spin is repeated with all conditions the same, except that the heater and extension are removed, filaments having a birefringence of about 0.0051 are obtained.
  • the heater has a plain metal tube with a cross-section of a frustrum of a cone that extends about 16 inches below the bottom of the heater.
  • the outer surface of the heater proper and the extension are well insulated.
  • the total distance below the spinneret in which the cooling rate is controlled is 24 inches.
  • Molten poly(ethylene terephthalate) is extruded from a pool at 310 C. through the spinneret of Example IV.
  • the extruded filaments pass directly through the heater.
  • Inert gas at the rate of about 7 cubic feet per minute C.
  • the resistance heaters are adjusted to give a gas temperature adjacent the spinneret of about 320 C.
  • the temperature profile within the heater is given in Table 3, item 8.
  • the threadline then passes over a finish roll where a lubricating finish is applied, and then around an unheated feed roll operating at a speed of about 500 yards per minute. Samples of yarn taken at this point have a birefringence of 0.0007 and a relative viscosity of 50.
  • the threadline From the feed roll the threadline next passes through a steam jet where steam at a temperature of 350 C. is impinged on the threadline to heat the yarn and establish a draw point. From the steam jet the yarn passes to and around a cold draw roll operating at a speed sufficient to give a draw ratio of 6.0. The threadline then passes to a conventional windup. The drawn yarn has a tenacity of 9.2 g.p.d. and a break elongation of 13%.
  • Example VI This example shows the more stringent conditions required to process higher molecular weight polyesters.
  • the heater is 6 inches long and consists of 3 concentric metal tubes, top and bottom walls.
  • the innermost tube of 9.2-inch inside diameter extends from the bottom wall to about 1 inch from the top, the middle tube extends from the top wall to about l inch from the bottom.
  • the outer tube contains electrical heaters on its inner wall and is insulated on the outside.
  • Preheated gas at a rate of 4.6 s.c.f.m. i.e., cubic feet per minute calculated for standard conditions of C. and 1 at-m.
  • enters the outermost plenum is distributed by the baflles and enters the innermost space.
  • Both plenum chambers containa thermocouple and the heaters are adjusted so that both thermocouples are at the same temperature.
  • the heater is separated from the spinning block by a 2-inch long insulator tube.
  • a 30-inch long insulated metal tube of 9.2-inch inside diameter is attached below the heater.
  • the Denier C is the ratio, 100 a/average diameter, where a is the standard deviation of the diameters of different filaments in the yarn and represents the uniformity of the yarn.
  • the percent Uster value is a measure of the uniformity V of denier along the length of a yarn.
  • Item ((1) which uses gas temperatures greater than the limits of this invention is significantly less uniform than item (c).
  • Example VII This example shows the effects of excessive heating of filaments.
  • Molten poly(ethylene terephtha'late) is extruded, from a 300 C. melt at a pressure averaging about 6200 p.s.i. through a spinneret, at 317 C. (calculated) into a heater similar to that of Example VI but having a 16"-long insulated metal extension tube, over a finish roll and a feed roll running at 385 to 387 y.p.m. The yarn is then quenched and drawn in a steam jet.
  • Results are given in Table 5.
  • the gas temperatures given have been calculated, using the temperature of the block, the polymer throughout, the hot gas temperature Example VIII is approximately the same as the poly(hexamethyland flow rate.
  • Items (a) and (b) are extruded through ene)adipamide component or about 2700 and 4100 poises 13 at 295 C. (T +30 C.) for shear rates of up to 10 secondsfor 70 RV and 80 RV, respectively.
  • the polymer is extruded from a pool at 282 C. through a spinneret containing 140 orifices of 12 mil diameter.
  • Example IX Lruded filaments pass through a 2.75-inch long recess in the spinning block, through the controlled heating zone, A polyarmde P p from (p y through a conventional chimney for rapid cooling of the heXyDmeihahe (Containing 90% 05 trails-(Tells configurafilaments, over a ceramic guide, a conventional finish roll, iiehs) and dedeeahedieie acid is used- The P y flake and to a feed roll (3 wraps) where samples of the as-spun has afeiaiive Viscosity 0f 7 as measured in 98% filaments are taken for birefringence determinations.
  • the formic acid/Phenol, 50150 y Weight at and has a filament bundle is passed from the feed roll to a two'stage crystalline melting Point Of drawing process consisting of 2 snubbing pins at 80 C.,
  • the p y is extruded from a melt at at a first draw roll (for 3.5x draw), a hot tube at 200 C. about 7000 P- Pressure through a Spinneret (containing (1.5 wraps) along about 28 inches of its length, a second 5 orifices 0i 9 mil diameter) into a Zone heated y steam, draw roll, a hot roll at 215 and a relaxing roll to permit ihehee through a quenching Zone Provided y ambient 6% shrinkage between the hot roll and windup.
  • the controlled heating zone is provided by a radial the Outer surface of iiihe p heated at to gas diff f 4 125-i length and 974 inside 235 C. to the second state draw roll and then to a windup. ameter consisting of an inner screen, a plenum chamber
  • the total draw ratio is Varied from X to X to g and an entrance for preheated gas (essentially N and the desired elongationco t a t equivalent to 3 bi f t/ i t at 0
  • the heated zone consists of (1) a 0.5-inch resess in the C. and 1 atmosphere.
  • An 8-inch long metal tube of conical spinning block all insulated metal tube 0f conical shape is attached to the bottom f th diff Th b tion with an inside diameter of 4 inches at the block and is shaped at a 30 angle to the vertical and is truncated an inside diameter of 6 inches at the bottom, a radial from 8 inches vertical distance in the back to 4.25 inches steam diihlsei" consisting of a e-iiieh inside diameter meiai vertical distance in the front.
  • the T temperatur tribution wall and an outer concentric chamber containing of the gas for the first 3.75 inches must vary between eieeiiieai heating eiemehis and an entrance for p the temperature of the spinning block (290 C.) and the heated steam, a metal Cone of 3-i11eh altitude With a fi t measured temperature base diameter of 6 inches, and (5) a metal tube of 3-inch
  • the temperature of the gas (T adj t t th inside diameter connected to the apex of the cone and exthreadline is measured by an aspirating thennccouple tending 28 lIlChfJS from it.
  • the as-spun fiber has a denier per filament of about 36 d.p.f.
  • the spin-stretch ratio is thus about 11.
  • the yarns for all items have an RV of 138, which polymer has a melt viscosity of about 25,000 poises at 330 C. and at a shear rate of up to 0.1 second
  • the great reduction in birefringence of the as-spun yarns of items (a) to (d) over the control item (e) is apparent.
  • the control yarn (item e) is drawn to give a tenacity of 5.4 g.p.d. at 11.7% elongation.
  • the yarn tenacities of items (a) to (d) range from 6.4 to 7.0 g.p.d.
  • the heated zone is provided by a l2-inch long 4-inch inside diameter, metal tube which has electrical heaters on its exterior, and is well insulated, and is held in place beneath and close to the spinneret.
  • Filaments are spun under 2 heating conditions, (B) and (C), (with medium and high heater control settings, respectively), and under one control condition (A) with the hot tube removed and replaced by the radial air quench.
  • Temperature profiles of the conditions (in C.) are given below.
  • the time (t in seconds 100) to reach 11 inches is 12.1, 6.0 and 4.0 for 150, 3 and 455 y.p.m., respectively.
  • Example X Commerc1a1 1sotact1c polypropylene of the following Gas Temperature Pwfile propert1es is used: Distance (inches) A B 0 Melt Index at Melt Flow Rate Viscosity Polymer 190 C./2,160 g. 230 C./2,160 g. (poiscs) AT AT AT at 200 C.
  • the synthetic organic polymer is a high molecular weight polyrner having a melt viscosity (7 of at least 5000 poises selected from the class consisting of polyesters, polyamides and polypropylene.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
US554620A 1960-04-29 1966-05-04 Melt-spinning process Expired - Lifetime US3361859A (en)

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Cited By (51)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3504078A (en) * 1967-09-29 1970-03-31 Du Pont Melt spinning process
US3512214A (en) * 1965-07-08 1970-05-19 Fuji Spinning Co Ltd Apparatus for melt spinning of synthetic filaments
US3536804A (en) * 1967-12-19 1970-10-27 Toyo Boseki Process for producing polyxyleneadipamide fibers
US3539676A (en) * 1966-08-29 1970-11-10 Celanese Corp Process for producing filaments and films of polymers of alkylene sulfides
US3549741A (en) * 1967-10-30 1970-12-22 Mildred H Caison Process for preparing improved carpet yarn
US3624193A (en) * 1969-02-25 1971-11-30 Du Pont Polyamide filamentmaking process including solid-state polymerization
US3645085A (en) * 1969-11-13 1972-02-29 Chemcell Ltd Hairy lustrous yarn
US3832436A (en) * 1972-04-06 1974-08-27 Ici Ltd Process for spinning high tenacity fibres
DE2447322A1 (de) * 1973-10-03 1975-04-17 Nat Res Dev Verfahren zur herstellung eines polymermaterials mit hohem modul
US3895090A (en) * 1968-04-09 1975-07-15 Asahi Chemical Ind Method for direct spinning of polyethylene-1,2-diphenoxyethane-p,p{40 -dicarboxylate fibers
US3963678A (en) * 1974-06-17 1976-06-15 E. I. Du Pont De Nemours And Company Large denier polyethylene terephthalate monofilaments having good transverse properties
US3969462A (en) * 1971-07-06 1976-07-13 Fiber Industries, Inc. Polyester yarn production
US3975488A (en) * 1972-10-24 1976-08-17 Fiber Industries, Inc. Process for preparing poly(tetramethylene terephthalate) yarn
US3998920A (en) * 1971-12-14 1976-12-21 Hoechst Aktiengesellschaft Process for the manufacture of tire monofilaments
US4000239A (en) * 1971-12-13 1976-12-28 Teijin Limited Process for spinning naphthalate polyester fibers
US4043985A (en) * 1971-12-14 1977-08-23 Hoechst Aktiengesellschaft Tire monofilaments
US4045534A (en) * 1974-05-24 1977-08-30 Allied Chemical Corporation Process for melt-spinning synthetic fibers
US4070432A (en) * 1975-02-13 1978-01-24 Allied Chemical Corporation Production of low shrink polyester fiber
DE2747803A1 (de) * 1976-10-26 1978-04-27 Celanese Corp Verfahren zur herstellung von verbesserten polyesterfilamenten hoher festigkeit und ungewoehnlich stabiler innerer struktur
DE2747690A1 (de) * 1976-10-26 1978-04-27 Celanese Corp Hochleistungs-polyesterfilamentgarn
US4096226A (en) * 1972-01-03 1978-06-20 Basf Aktiengesellschaft Integrated spin-draw-texturizing process for manufacture of texturized polyamide filaments
US4113821A (en) * 1971-09-23 1978-09-12 Allied Chemical Corporation Process for preparing high strength polyamide and polyester filamentary yarn
US4193961A (en) * 1978-04-04 1980-03-18 Kling-Tecs, Inc. Method of extruding polypropylene yarn
US4195161A (en) * 1973-09-26 1980-03-25 Celanese Corporation Polyester fiber
US4204828A (en) * 1978-08-01 1980-05-27 Allied Chemical Corporation Quench system for synthetic fibers using fog and flowing air
US4228118A (en) * 1977-11-03 1980-10-14 Monsanto Company Process for producing high tenacity polyethylene fibers
US4268470A (en) * 1975-11-05 1981-05-19 National Research Development Corporation Polymer materials
US4303606A (en) * 1978-04-04 1981-12-01 Kling Tecs, Inc. Method of extruding polypropylene yarn
US4338275A (en) * 1977-08-19 1982-07-06 Imperial Chemical Industries Limited Process for the manufacture of polyester yarns
US4338276A (en) * 1977-08-19 1982-07-06 Imperial Chemical Industries, Ltd. Process for the manufacture of polyamide yarns
EP0059418A1 (fr) * 1981-02-26 1982-09-08 Asahi Kasei Kogyo Kabushiki Kaisha Fibre de nylon 66 susceptible de se teindre uniformément et procédé pour sa production
US4359557A (en) * 1980-09-11 1982-11-16 Eastman Kodak Company Process for producing low pilling textile fiber and product of the process
US4384098A (en) * 1981-01-13 1983-05-17 Phillips Petroleum Company Filamentary polypropylene and method of making
US4415522A (en) * 1974-03-05 1983-11-15 National Research Development Corporation Process for the continuous production of high modulus filament of polyethylene
US4522773A (en) * 1983-02-24 1985-06-11 Celanese Corporation Process for producing self-crimping polyester yarn
US4539170A (en) * 1983-09-26 1985-09-03 E. I. Du Pont De Nemours And Company Process for steam-conditioning spin-oriented polyamide filaments
US4758472A (en) * 1982-07-08 1988-07-19 Asahi Kasei Kogyo Kabushiki Kaisha High tenacity polyhexamethylene adipamide fiber
US5049339A (en) * 1989-07-03 1991-09-17 The Goodyear Tire & Rubber Company Process for manufacturing industrial yarn
US5108675A (en) * 1982-05-28 1992-04-28 Asahi Kasei Kogyo Kabushiki Kaisha Process for preparing easily dyeable polyethylene terephthalate fiber
US5171504A (en) * 1991-03-28 1992-12-15 North Carolina State University Process for producing high strength, high modulus thermoplastic fibers
US5182068A (en) * 1990-05-22 1993-01-26 Imperial Chemical Industries Plc High speed spinning process
US5186879A (en) * 1990-05-11 1993-02-16 Hoechst Celanese Corporation Spinning process for producing high strength, high modulus, low shrinkage yarns
US5238740A (en) * 1990-05-11 1993-08-24 Hoechst Celanese Corporation Drawn polyester yarn having a high tenacity and high modulus and a low shrinkage
US5279783A (en) * 1992-01-30 1994-01-18 United States Surgical Corporation Process for manufacture of polyamide monofilament suture
US5349044A (en) * 1992-01-30 1994-09-20 United States Surgical Corporation Polyamide monofilament suture manufactured from higher order polyamide
US5352518A (en) * 1990-06-22 1994-10-04 Kanebo, Ltd. Composite elastic filament with rough surface, production thereof, and textile structure comprising the same
US5629080A (en) * 1992-01-13 1997-05-13 Hercules Incorporated Thermally bondable fiber for high strength non-woven fabrics
US5882562A (en) * 1994-12-19 1999-03-16 Fiberco, Inc. Process for producing fibers for high strength non-woven materials
WO2007059914A1 (fr) * 2005-11-24 2007-05-31 Oerlikon Textile Gmbh & Co. Kg Procede et dispositif pour filer a chaud et refroidir un brin multifilaire avec mesure de la temperature de l'air de refroidissement a l'interieur du faisceau de filaments
US9447522B2 (en) 2011-09-02 2016-09-20 Aurotec Gmbh Extrusion method
US11746443B1 (en) 2019-06-07 2023-09-05 Cook Biotech Incorporated Polycaprolactone-based fibers and implants including same

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US3291880A (en) * 1964-12-23 1966-12-13 Du Pont Process for preparing an undrawn, low birefringence polyamide yarn
EP0041327B1 (fr) * 1980-05-30 1983-09-07 Imperial Chemical Industries Plc Procédé de filage au fondu
US4352400A (en) * 1980-12-01 1982-10-05 Christensen, Inc. Drill bit
EP0200472B1 (fr) * 1985-04-23 1990-12-05 Teijin Limited Fibres et fibres conjugées de polyamides entièrement aromatiques, leur procédé de production et leur utilisation

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US3512214A (en) * 1965-07-08 1970-05-19 Fuji Spinning Co Ltd Apparatus for melt spinning of synthetic filaments
US3539676A (en) * 1966-08-29 1970-11-10 Celanese Corp Process for producing filaments and films of polymers of alkylene sulfides
US3504078A (en) * 1967-09-29 1970-03-31 Du Pont Melt spinning process
US3549741A (en) * 1967-10-30 1970-12-22 Mildred H Caison Process for preparing improved carpet yarn
US3536804A (en) * 1967-12-19 1970-10-27 Toyo Boseki Process for producing polyxyleneadipamide fibers
US3895090A (en) * 1968-04-09 1975-07-15 Asahi Chemical Ind Method for direct spinning of polyethylene-1,2-diphenoxyethane-p,p{40 -dicarboxylate fibers
US3624193A (en) * 1969-02-25 1971-11-30 Du Pont Polyamide filamentmaking process including solid-state polymerization
US3645085A (en) * 1969-11-13 1972-02-29 Chemcell Ltd Hairy lustrous yarn
US3969462A (en) * 1971-07-06 1976-07-13 Fiber Industries, Inc. Polyester yarn production
US4113821A (en) * 1971-09-23 1978-09-12 Allied Chemical Corporation Process for preparing high strength polyamide and polyester filamentary yarn
US4000239A (en) * 1971-12-13 1976-12-28 Teijin Limited Process for spinning naphthalate polyester fibers
US3998920A (en) * 1971-12-14 1976-12-21 Hoechst Aktiengesellschaft Process for the manufacture of tire monofilaments
US4043985A (en) * 1971-12-14 1977-08-23 Hoechst Aktiengesellschaft Tire monofilaments
US4096226A (en) * 1972-01-03 1978-06-20 Basf Aktiengesellschaft Integrated spin-draw-texturizing process for manufacture of texturized polyamide filaments
US3832436A (en) * 1972-04-06 1974-08-27 Ici Ltd Process for spinning high tenacity fibres
US3975488A (en) * 1972-10-24 1976-08-17 Fiber Industries, Inc. Process for preparing poly(tetramethylene terephthalate) yarn
US4195161A (en) * 1973-09-26 1980-03-25 Celanese Corporation Polyester fiber
DE2447322A1 (de) * 1973-10-03 1975-04-17 Nat Res Dev Verfahren zur herstellung eines polymermaterials mit hohem modul
US4287149A (en) * 1973-10-03 1981-09-01 National Research Development Corp. Process for the production of polymer materials
US4415522A (en) * 1974-03-05 1983-11-15 National Research Development Corporation Process for the continuous production of high modulus filament of polyethylene
US4045534A (en) * 1974-05-24 1977-08-30 Allied Chemical Corporation Process for melt-spinning synthetic fibers
US3963678A (en) * 1974-06-17 1976-06-15 E. I. Du Pont De Nemours And Company Large denier polyethylene terephthalate monofilaments having good transverse properties
US4070432A (en) * 1975-02-13 1978-01-24 Allied Chemical Corporation Production of low shrink polyester fiber
US4647640A (en) * 1975-11-05 1987-03-03 National Research Development Corporation Polymer materials
US4268470A (en) * 1975-11-05 1981-05-19 National Research Development Corporation Polymer materials
US4525564A (en) * 1975-11-05 1985-06-25 National Research Development Corporation High modulus, low creep strain polyalkene polymer materials
DE2747690A1 (de) * 1976-10-26 1978-04-27 Celanese Corp Hochleistungs-polyesterfilamentgarn
US4195052A (en) * 1976-10-26 1980-03-25 Celanese Corporation Production of improved polyester filaments of high strength possessing an unusually stable internal structure
DE2747803A1 (de) * 1976-10-26 1978-04-27 Celanese Corp Verfahren zur herstellung von verbesserten polyesterfilamenten hoher festigkeit und ungewoehnlich stabiler innerer struktur
US4338276A (en) * 1977-08-19 1982-07-06 Imperial Chemical Industries, Ltd. Process for the manufacture of polyamide yarns
US4338275A (en) * 1977-08-19 1982-07-06 Imperial Chemical Industries Limited Process for the manufacture of polyester yarns
US4228118A (en) * 1977-11-03 1980-10-14 Monsanto Company Process for producing high tenacity polyethylene fibers
US4303606A (en) * 1978-04-04 1981-12-01 Kling Tecs, Inc. Method of extruding polypropylene yarn
US4193961A (en) * 1978-04-04 1980-03-18 Kling-Tecs, Inc. Method of extruding polypropylene yarn
US4204828A (en) * 1978-08-01 1980-05-27 Allied Chemical Corporation Quench system for synthetic fibers using fog and flowing air
US4359557A (en) * 1980-09-11 1982-11-16 Eastman Kodak Company Process for producing low pilling textile fiber and product of the process
US4384098A (en) * 1981-01-13 1983-05-17 Phillips Petroleum Company Filamentary polypropylene and method of making
EP0059418A1 (fr) * 1981-02-26 1982-09-08 Asahi Kasei Kogyo Kabushiki Kaisha Fibre de nylon 66 susceptible de se teindre uniformément et procédé pour sa production
US5108675A (en) * 1982-05-28 1992-04-28 Asahi Kasei Kogyo Kabushiki Kaisha Process for preparing easily dyeable polyethylene terephthalate fiber
US4758472A (en) * 1982-07-08 1988-07-19 Asahi Kasei Kogyo Kabushiki Kaisha High tenacity polyhexamethylene adipamide fiber
US4522773A (en) * 1983-02-24 1985-06-11 Celanese Corporation Process for producing self-crimping polyester yarn
US4539170A (en) * 1983-09-26 1985-09-03 E. I. Du Pont De Nemours And Company Process for steam-conditioning spin-oriented polyamide filaments
US5049339A (en) * 1989-07-03 1991-09-17 The Goodyear Tire & Rubber Company Process for manufacturing industrial yarn
US5186879A (en) * 1990-05-11 1993-02-16 Hoechst Celanese Corporation Spinning process for producing high strength, high modulus, low shrinkage yarns
US5238740A (en) * 1990-05-11 1993-08-24 Hoechst Celanese Corporation Drawn polyester yarn having a high tenacity and high modulus and a low shrinkage
US5182068A (en) * 1990-05-22 1993-01-26 Imperial Chemical Industries Plc High speed spinning process
US5352518A (en) * 1990-06-22 1994-10-04 Kanebo, Ltd. Composite elastic filament with rough surface, production thereof, and textile structure comprising the same
US5171504A (en) * 1991-03-28 1992-12-15 North Carolina State University Process for producing high strength, high modulus thermoplastic fibers
US5629080A (en) * 1992-01-13 1997-05-13 Hercules Incorporated Thermally bondable fiber for high strength non-woven fabrics
US5654088A (en) * 1992-01-13 1997-08-05 Hercules Incorporated Thermally bondable fiber for high strength non-woven fabrics
US5733646A (en) * 1992-01-13 1998-03-31 Hercules Incorporated Thermally bondable fiber for high strength non-woven fabrics
US5888438A (en) * 1992-01-13 1999-03-30 Hercules Incorporated Thermally bondable fiber for high strength non-woven fabrics
US5349044A (en) * 1992-01-30 1994-09-20 United States Surgical Corporation Polyamide monofilament suture manufactured from higher order polyamide
US5405358A (en) * 1992-01-30 1995-04-11 United States Surgical Corporation Polyamide monofilament suture
US5540717A (en) * 1992-01-30 1996-07-30 U.S. Surgical Corporation Polyamide monofilament suture manufactured from higher order polyamide
US5279783A (en) * 1992-01-30 1994-01-18 United States Surgical Corporation Process for manufacture of polyamide monofilament suture
US5882562A (en) * 1994-12-19 1999-03-16 Fiberco, Inc. Process for producing fibers for high strength non-woven materials
WO2007059914A1 (fr) * 2005-11-24 2007-05-31 Oerlikon Textile Gmbh & Co. Kg Procede et dispositif pour filer a chaud et refroidir un brin multifilaire avec mesure de la temperature de l'air de refroidissement a l'interieur du faisceau de filaments
CN101313090B (zh) * 2005-11-24 2010-12-08 欧瑞康纺织有限及两合公司 用于熔纺和冷却复丝的方法和设备
US9447522B2 (en) 2011-09-02 2016-09-20 Aurotec Gmbh Extrusion method
US11746443B1 (en) 2019-06-07 2023-09-05 Cook Biotech Incorporated Polycaprolactone-based fibers and implants including same

Also Published As

Publication number Publication date
NL264104A (fr)
GB900009A (en) 1962-07-04
IT650394A (fr)
CA697541A (en) 1964-11-10
DE1435614A1 (de) 1969-12-04
FR1287939A (fr) 1962-03-16

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