US3414646A - Coupled process for the production of polycarbonamide filaments - Google Patents

Coupled process for the production of polycarbonamide filaments Download PDF

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Publication number
US3414646A
US3414646A US451822A US45182265A US3414646A US 3414646 A US3414646 A US 3414646A US 451822 A US451822 A US 451822A US 45182265 A US45182265 A US 45182265A US 3414646 A US3414646 A US 3414646A
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United States
Prior art keywords
yarn
filaments
filament
temperature
steaming
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US451822A
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English (en)
Inventor
Pitzl Gilbert
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EIDP Inc
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EI Du Pont de Nemours and Co
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Application filed by EI Du Pont de Nemours and Co filed Critical EI Du Pont de Nemours and Co
Priority to US451822A priority Critical patent/US3414646A/en
Priority to NL6605119A priority patent/NL6605119A/xx
Priority to LU50975A priority patent/LU50975A1/xx
Priority to DE19661660570 priority patent/DE1660570B2/de
Priority to GB1887066A priority patent/GB1093871A/en
Application granted granted Critical
Publication of US3414646A publication Critical patent/US3414646A/en
Priority to US864256A priority patent/US3550369A/en
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Expired - Lifetime legal-status Critical Current

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    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02JFINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/22Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
    • D02J1/221Preliminary treatments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D11/00Other features of manufacture
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/08Melt spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides

Definitions

  • ABSTRACT OF THE DISCLOSURE A coupled process for the production of polycarbonamide filaments which includes extruding, quenching in a gaseous non-aqueous atmosphere, treating with steam while the temperature of the filaments is in the range of T to T +60 C., then drawing. T is the force-todraw transition temperature of the filaments.
  • This invention relates to improved nylon yarn and a process for its production.
  • nylon yarn is usually produced by melt-spinning polyamide filaments, winding the undrawn yarn into a package, and subsequently unwinding and drawing the yarn. Due to the separation of the spinning and drawing steps, this practice may be termed a split process.
  • Split process yarns are usually subjected to a steam treatment as taught by Babcock in US. 2,289,- 860 to provide satisfactory package formation on winding the undrawn yarn.
  • Coupled-process filaments tend to have a very smooth surface which, in turn, leads to high yarn-to-guide friction in processing the yarn into fabrics. This high level of friction results in higher and more variable tension which in turn causes undesirable non-uniformities such as streaks in the fabric.
  • This diificulty is avoided with split process yarns by aging the undrawn yarn for several hours before drawing. The surface roughness of the filaments is appreciably increased by this procedure.
  • a coupled-process for the continuous production of drawn synthetic polymer filaments from a melt of a polycarbonamide by the sequential steps of extruding said melt in the form of filaments, at least partially quenching the melt in a gaseous, non-aqueous cooling medium to solidify the filaments and then drawing the filaments to at least twice their as-spun length; the improvement comprising intermediate said quenching and drawing steps treating the filaments with steam while their surface temperature is in the range of T to T +60 C.,'wherein T is the force-to-draw transition temperature of the filaments.
  • the novel product of the invention is a low friction yarn comprising synthetic polymer filaments of a polycarbonamide, said filaments being characterized by a rough texture on their surface and, as viewed in electron micrographs of shadowed cross-sections, as having a smooth central portion surrounded by a rough, grainy peripheral area. This structure will be best understood by reference to the photomicrographs to be described hereinafter.
  • FIGURE 1 shows photomicrographs of filament crosssections, that of A being a product of the invention and B and C being prior art products;
  • FIGURE 2 shows photomicrographs of filament surfaces, that of A being a product of the invention and B and C being prior art products;
  • FIGURE 3 is a schematic drawing showing the various steps of the process of the present invention.
  • FIGURE 4 is a graph, to be explained in connection with Example 2, showing the effect upon tension when the filament surface temperature is varied in the steaming step.
  • filaments 1 freshly extruded from spinneret 2 pass into cooling chimney 3 where they are contacted by cross flow air 4.
  • Convergence guide 5 adjustable in position to assist control of filament temperature, leads the yarn at the desired temperature out of chimney 3 and into steamer 6 where a cross flow of steam 7 contacts the still hot filaments.
  • finish roller 8 After passing out of steamer 6, the yarn passes over finish roller 8 to apply a lubricating finish and then around a pair of rolls 10.
  • the yarn is continuously drawn by wraps around a pair of heated rolls 12 moving at higher speed.
  • the yarn then passes over driven roll 13 and finally advances through guide 15 to a package 20 where it is wound on cylindrical core 21 which is surface driven by drive roll 22.
  • the process of this invention in particular the application of steam to the filaments at a critical period in the consolidation of their structure, promotes crystal growth at and near the filament surface and as a result a very rough, bumpy surface, as illustrated in FIGURE 2-A, is formed when the yarn is drawn. Unlike splitprocess yarns, however, this effect does not extend throughout the filament cross-section and, as a consequence, the improved properties of the yarn relativeto split-process yarn are retained.
  • a nucleating agent such as the kaolinite particles exemplified hereinafter or other finely divided particulate material
  • spherulites are formed near the filament surface when the yarn is steamed in accordance with this invention and this leads to a somewhat rougher surface than obtained with steaming alone.
  • spherulites are crystalline aggregates of more or less spherical shape which form when certain polymer melts are cooled.
  • Excessive spherulitic growth i.e., throughout the filament cross-section, is undesirable from the standpoint of obtaining optimum fiber properties and is usually avoided by rapid cooling of the extruded filaments to a temperature below the glassor second-order transition temperature which is referred to herein as the force-todraw transition temperature.
  • the desired filamentsurface roughening is not achieved.
  • the initial modulus of the yarn is indicative of the rate at which the yarn elongates with increasing load in the early stages of elongation. Practically, it is determined from the stress-strain curve by multiplying the load in grams at 1% elongation on the loading curve by 100 and dividing by the denier of the yarn.
  • Measurements of yarn friction as reported herein are made by passing the yarn at 250 y.p.m. (228.5) meters/ min.) over 21% inch (9.5 mm.) diameter polished chrome pin. The yarn contacts the pin over an angle of 164 C.
  • the yarn is passed from a supply package over a magnetic brake to apply the desired tension, then downwardly to and around a small pulley attached to a Statham strain gauge. From the pulley, the yarn is passed up and over the chrome pin and then down to a second pulley attached to another strain gauge. From the second pulley, the yarn is passed upwardly to a powerdriven roller and an associated idler roller where it is given several passes around these rollers to avoid slippage.
  • the yarn is passed from the power-driven roller to an aspirator which carries the yarn to a waste container.
  • the input tension, T is adjusted to 10 grams as measured on the first strain gauge.
  • the output tension, T is measured by the second strain gauge, the strain gauges being connected to suitable recorders for this purpose.
  • the output tension developed may be compared when the input tension is constant.
  • the coefiicient of friction 1 may be calculated from the equation wherein T is the input tension, T the output tension, 12 is the angle of yarn contact in radians and e is the base of the natural log.
  • the values for force-to-draw transition temperatures are determined by measurin the force-to-draw at different yarn temperatures and plotting a curve of force-to-draw vs. yarn temperature. The lowest temperature above room temperature at which a definite break in the curve is observed is taken as the transition temperature for the particular yarn. Since the force-todraw transition temperature for nylon varies with the degree of crystallinity, orientation and moisture content, the force-to-draw is determined by passing yarn directly after quenching to a heated feed roll of 6.72 inches (17 cm.) diameter, passing the yarn around the feed roll for 16 turns to insure temperature equilibration, then passing the yarn to a draw roll and drawing to a 2.2 draw ratio. The force-to-draw transition temperature of the 66 nylon yarns referred to herein is about 59 C in all cases.
  • the surface temperature of the filaments is determined with a compensating thermocouple arrangement in which one of a pair of thermocouples is placed in contact with the running filament and the other thermocouple is heated electronically until the two are in balance.
  • a commercially available instrument of this type and manufactured by the Hastings-Radist Company was used in measuring the filament temperatures reported herein.
  • the rate and depth of dyeing of yarns are determined using an aqueous solution of anthraquinone blue SWF at a concentration of 1% based on the weight of the yarn to be immersed in the dye bath and a temperature of C.
  • the depth of dyeing is reported in terms of the number of shades difference in depth of one sample relative to another. Plus signs indicate deeper dyeing, while minus signs indicate slighter dyeing.
  • the rate of dyeing is calculated on a basis of the percent dye, based on the weight of the yarn, taken up in a unit of time.
  • the filament is embedded in a copolymer of methyl and butyl methacrylate.
  • Cross sections of 0.3-0.5 micron thickness are then cut using a microtome with a glass knife. Knives other than glass, particularly diamond, should be avoided.
  • the embedded filament cross-section is then placed on a metal grid or screen and placed under a bell jar where a high vacuum is created.
  • a mixture of gold and palladium is then deposited on the cross section from a heated goldpalladium filament mounted at an angle with respect to the surface of the filament cross-section. If the surface of the cross-section is completely smooth, an even coating of the metal results.
  • cross-section is rough or irregular, then more metal is deposited on the side adjacent the heated metal filament and an irregular coating results.
  • the cross-section is then examined in the electron microscope and an electron micrograph prepared using conventional techniques with the electron beam perpendicular to the surface of the filament.
  • the filament is mounted on a microscope slide, placed in vacuum and exposed to metal vaporization at an angle to the surface of the filament following the procedure described above for shadowed cross sections.
  • the filament is then dipped in polyacrylic acid to embed one side.
  • the slide is removed, leaving the metal-coated filament with one side (the metalcoated side) embedded in the hardened polyacrylic acid.
  • the filament is then peeled out of the metal coating which remains adhered to the polyacrylic acid.
  • the polyacrylic acid is then dissolved with water and an electron micrograph made of the metal surface replica.
  • the yarn is then passed over a finish roller where a lubricating finish is applied, then around a feed roller and its associated idler roller, then around a draw roller having a sufficiently higher peripheral speed than the feed roller to draw the yarn to a ratio of 3.2.
  • the draw roller is located in a heated compartment having an air temperature of C. and the peripheral speed of the draw roller is 3,500 y.p.m.
  • the yarn is passed around a second roller in the heated compartment and then back around the draw roller, the second roller having the same peripheral speed as the draw roller so that the yarn is subjected to a constant-length heat treatment.
  • the yarn then passes from the heated compartment directly to and around a roller having a lower peripheral speed to permit the yarn to retract slightly and thereby reduce the winding tension.
  • the yarn is then passed to a rotating bobbin where it is Wound into a package in the conventional manner.
  • FIGURE lA An electron micrograph of a replica of the filament surface shows it to be rough and bumpy as illustrated in FIGURE 2-A.
  • FIGURES 1-B and 2-B are illustrated, respectively, in FIGURES 1-B and 2-B.
  • the entire cross section is smooth and the surface EX MP E II of the filament is smooth relative to the steamed filament.
  • FIGURES 1-C and 2C Electron micrographs of a shadowed cross section and a filament surface replica are prepared and illustrated in FIGURES 1-C and 2C. As can be seen from these figures, the rough, grainy structure appears throughout the shadowed cross section and the surface, although rough and striated, appears smoother than that of the yarn of this invention. Shadowed cross sections and surface replicas are also prepared from split process yarns which have been aged for more than 8 hours before drawing and are found to be identical with those of FIGURES l-C and 2-C.
  • the yarn of this invention i.e., the coupled-process steamed yarn
  • the co-efiicient of friction of the yarn of this invention is substantially lower than either of the other two.
  • the yarn of this invention When the yarn of this invention is used as a filling in a fabric having a conventional 70-denier nylon warp, the quilling tension being 20 grams, the quill barr is judged to be at an acceptable level. Under the same conditions, the unsteamed coupled-process yarn produces 35 grams quilling tension and an unacceptable level of quill barr.
  • EXAMPLE II coupled-process yarns of various filament deniers are prepared as in Example I except that the temperature of the yarn at the point of steaming, i.e., as the yarn enters the steamer, is varied in the range 45-90 C., by changing the location of the steamer or the convergence guide.
  • the output tension varies with the temperature of the yarn at steaming as shown by the curve in FIGURE ultra flotation process (US. Patent No.
  • 2,990,958 to substantially eliminate metal oxides other than aluminum and silicon oxide and classified by centrifugation to provide an average maximum dimension of 0.55 micron, are mixed with 300 parts water and 1.2 parts tetrasodiumpyrophosphate decahydrate in a high-shear mixing mill. After milling for 1 hour, the mixture is diluted with 300 parts water, transferred to a tank and stirred for 24 hours. The slurry is allowed to settle for 20 hours, then decanted from the settled materials and diluted with water to a concentration of 20% solids. The diluted slurry is then passed through a standard commercial filter having an average pore size of 5 microns and continuously stirred until used.
  • the product of this invention has a structure such that when examined microscopically at a magnification of at least 1600 the outer surface of the filament is rough to provide low yarn to guide friction which is needed in textile processing operations, while the internal or core structure is apparently unchanged so that advantages in strength and modulus are retained. Also, even though the outer portion of the filament cross section is changed, the enhanced dyeability of the coupled filament is retained.
  • This desirable structure is obtained by steaming the filaments at a temperature above the force-to draw transition temperature.
  • the temperature of the filaments as they enter the steaming zone is at least C.
  • the temperature should not exceed the softening temperature of the filaments.
  • the temperature of the filaments should be in the range of 540 C. above the force-to-draw transition temperature.
  • the preferred temperature range for 66 nylon is 65-1 00" C.
  • the temperature referred to is, in all cases, the surface temperature of the filaments, since this is the only temperature which can be measured practically.
  • the yarns of this invention may be prepared from any polyamide which crystallizes readily in the presence of heat and moisture.
  • the preferred polyamides are 66 and 6 nylon; that is, poly(hexamethylene adipamide) and poly(epsiloncaproamide), respectively.
  • Other suitable polyamides for this purpose are those disclosed in US. Patents 2,071,253, 2,130,523 and 2,130,948.
  • the duration of steaming is not highly critical; however, for reasons of economy and operability, steaming times in the range of 0.0040.02 second are preferred. Particularly with the shorter steaming periods, the steam should be applied uniformly and with minimum turbulence in order to prevent non-uniformities in the resulting filaments.
  • a steamer of the type disclosed and claimed in co-pending U.Sv application Ser. No. 420,547 filed Dec. 23, 1964, now US. Patent No. 3,316,741 is preferred.
  • the particular temperature and degree of saturation of the steam do not alfect the results obtained.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
US451822A 1965-04-29 1965-04-29 Coupled process for the production of polycarbonamide filaments Expired - Lifetime US3414646A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
US451822A US3414646A (en) 1965-04-29 1965-04-29 Coupled process for the production of polycarbonamide filaments
NL6605119A NL6605119A (OSRAM) 1965-04-29 1966-04-15
LU50975A LU50975A1 (OSRAM) 1965-04-29 1966-04-26
DE19661660570 DE1660570B2 (de) 1965-04-29 1966-04-29 Verfahren zur kontinuierlichen herstellung von faeden mit einer rauhen oberflaeche aus einer polycarbonsaeureamidschmelze
GB1887066A GB1093871A (en) 1965-04-29 1966-04-29 Filaments of drawn polycarbonamides
US864256A US3550369A (en) 1965-04-29 1969-09-10 Steamed coupled-process nylon yarn

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US451822A US3414646A (en) 1965-04-29 1965-04-29 Coupled process for the production of polycarbonamide filaments

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DE (1) DE1660570B2 (OSRAM)
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3679786A (en) * 1970-05-21 1972-07-25 Phillips Fibers Corp Method and apparatus for melt spinning of synthetic filaments
US4396570A (en) * 1981-05-01 1983-08-02 Allied Corporation Nylon spin-draw process with steam conditioning
DE4224453A1 (de) * 1991-08-02 1993-02-04 Barmag Barmer Maschf Verfahren zum herstellen eines hochfesten multifilen synthesegarnes
US5487860A (en) * 1992-03-30 1996-01-30 Basf Corporation Continuous process for spinning and drawing polyamide and apparatus thereof
US10968565B2 (en) * 2014-05-02 2021-04-06 Polytex Sportbeläge Produktions GmbH Artificial turf production using a nucleating agent

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2289860A (en) * 1938-08-09 1942-07-14 Du Pont Process and apparatus for the production of artificial fibers and the like
US3039171A (en) * 1960-06-09 1962-06-19 Du Pont Process of drawing filaments
US3291880A (en) * 1964-12-23 1966-12-13 Du Pont Process for preparing an undrawn, low birefringence polyamide yarn

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2289860A (en) * 1938-08-09 1942-07-14 Du Pont Process and apparatus for the production of artificial fibers and the like
US3039171A (en) * 1960-06-09 1962-06-19 Du Pont Process of drawing filaments
US3291880A (en) * 1964-12-23 1966-12-13 Du Pont Process for preparing an undrawn, low birefringence polyamide yarn

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3679786A (en) * 1970-05-21 1972-07-25 Phillips Fibers Corp Method and apparatus for melt spinning of synthetic filaments
US4396570A (en) * 1981-05-01 1983-08-02 Allied Corporation Nylon spin-draw process with steam conditioning
DE4224453A1 (de) * 1991-08-02 1993-02-04 Barmag Barmer Maschf Verfahren zum herstellen eines hochfesten multifilen synthesegarnes
US5487860A (en) * 1992-03-30 1996-01-30 Basf Corporation Continuous process for spinning and drawing polyamide and apparatus thereof
US10968565B2 (en) * 2014-05-02 2021-04-06 Polytex Sportbeläge Produktions GmbH Artificial turf production using a nucleating agent

Also Published As

Publication number Publication date
DE1660570B2 (de) 1976-08-12
LU50975A1 (OSRAM) 1966-06-27
DE1660570A1 (de) 1971-05-13

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