US2734794A - G cm-ton - Google Patents

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US2734794A
US2734794A US2734794DA US2734794A US 2734794 A US2734794 A US 2734794A US 2734794D A US2734794D A US 2734794DA US 2734794 A US2734794 A US 2734794A
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fibers
yarn
wool
range
temperatures
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    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S8/00—Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
    • Y10S8/04—Polyester fibers

Definitions

  • This invention relates to a process for preparing resil ient polyethylene terephthalate fibers and is particularly concerned with a process for producing polyethylene terephthalate fibers and yarn possessing desirable characteristics of fine wool.
  • a further object is to provide a process for preparing uniform, drawn polyethylene terephthalate fibers of woollike properties, which fibers will not be subject to additional cold drawing during subsequent normal processing.
  • polyethylene terephthalate fibers which have a birefringence in the range of 0.004 to 0.11 to 90% to 100% of the maximum draw ratio obtainable at temperatures in the range of 35 to 50 C. while the fibers are wet with a hydroxylated non-solvent, preferably water or a dilute aqueous solution.
  • the fiber-forming material is principally polyethylene"terephthalate but the inclusion therein of up to 10 mol per cent of modifying material is intended 'wheneverthe expression polyethylene terephthalate material is used.
  • Polyethylene terephthalate, itself, is a poly-condensation product of ethylene glycol and terephthalic acid or an ester-forming derivative thereof. During the preparation of this polyester, minor amounts of a modifying material may be added, for example, another glycol and/or'another dicarboxylic acid.
  • a'suitable funicular structure comprised essentially of polyethylene terephthalate may-have included in the polymer molecule up to 10 mol per cent of another glycol such asdieth ylene glycol,'tetramethylene glycol or hexamethylene glycol. Or again, the molecule may contain up to 10 mol per cent of another acid.
  • suitable examples of modifying acids there may be mentioned hexahydroterephthalic acid, bibenzoic acid, adipic acid,'sebacic acid, azelaic acid, the naphthalic acids, 2.5-dimethylterephthalic acid and bis-p-carboxyphenoxyethane.
  • modifiers may be added as one of the initial reactants during the polymerization process, but the modifying materials may also be polymerized-separately and then melt-blended with the polyethylene terephthalate. In either case, the total amount of modifier in the final polymeric material should not exceed 10 mol per cent.
  • the polyesters are suitably prepared as described in U. S. Patent 2,465,319.
  • the ethylene terephthalate polymer preferably has an intrinsic viscosity of at least 0.3. Those polymers :having lower intrinsic viscosities are essentially non-fiber forming.
  • the expression intrinsic viscosity is used herein as a measure of the degree of polymerization of the polyester and may be defined as limit s r as C approaches 0 and 5.0% for each determination.
  • the yarns and fibers prepared in accordance with the process of this invention possess a property of wool which is mostdifficult to duplicate, namely, resilience. This property is not easy to measure quantitatively, but may be defined to a considerable extent by three important parameters: Initial'tensile modulus, tensile recovery, and compliance ratio.
  • the initial tensile modulus (represented by the symbol M1 is defined as the slope of the first reasonably straight portion of a stress-strain curve of the funicular structure obtained by plotting tension on a vertical axis vs. elongation on a horizontal axis as the structure is being'elongatcd at the rate of per minute under standard conditions of temperature (21 C.) and humidity (60% RH). In almost every instance, this first reasonably straight portion is also'the steepest slope to be found on the curve.
  • the values as used herein are in units of kilograms per square millimeter per 100% elongation.
  • the initial tensile modulus, Mi is a measure of resistance to stretching and bending.
  • the effects of the filament modulus are felt in a fabric chiefly when the fabric is folded or crushed in the hand or otherwise handled. If the modulus is too low, the fabric is rubbery" or limp"; with too high a modulus in the fibers, the fabric is wiry or boardy. When the modulus is in the proper range, a soft fabric results. Attempts have been made to counteract the effects of a modulus lying outside the wool range by a suitable adjustment of filament diameter. In each instance, this straying away from the usual diameters of wool filaments has resulted 'in deleterious effects on properties such as liveliness and recovery from wrinkling.
  • the tensile recovery is defined as the extent to which the yarn recovers its original length after being stretched, a stress-strain curve being used to determine tensile recovery under the testing conditions.
  • the test consists in extending the funicular structure at a constant rate of elongation of 10% per minute. A specimen is held at the maximum elongation desired for 30 seconds, e. g., by the use ofa time switch, and is then allowed to retract at the same rate at which it was extended. The same specimen is extended approximately 1.0, 3.0 The extension during elongation and the recovery during retraction are measured along the elongation axis. The tensile recovery is then the ratio of the extent to which the yarn retracts to the extent to which it was elongated. This test is run under standard conditions at 60% RH and 21 C.
  • the tensile recovery correlates in a high degree with these properties.
  • the tensile recoveryfroma 1% elongation correlates with fabric recovery from mild wrinkling, and, as might be expected; the tensilerecoveryrfrom higher elongations correlates with recovery from rnore'severe wrinkling and In this instance, the words, resistance to may be used alternatively to recovery from?" since resistance to a crease or wrinkle really involves a very rapid and complete recovery from a crease or-wrinkle when the deforming force is removed.
  • the rapid recovery is a characteristic of the polyethylene terephthalate materials of this invention.
  • the .compliance ratio isessociated with the shape of a stress strain curvean'd'is atmeasure 'ofithe rate of change of compliance with elongation. Compliance is defined' as elongation divided by tension-in kg./mm. Hookean systems, those for which the stressstrain curve is a straight line, exhibit equal compliance at all elongations, and for these the change of compliance with elongation is 0.
  • one of the most important properties of wool is its change toward higher complianceas it is progressively deformed. Itis this property which enables wool to feel simultaneously crisp and soft. This property is measured by determining the average rate at which compliance changes in the range 5 to 10% elongation and is computed by the'following formula:
  • the stress-strain curve of wool has two distinctly different regions, consisting of (1) an initial portion in which the resistance to deformation is relatively great, and (2) a later portion in which the resistance decreases regularly and to a high degree. It is for this reason'that a'wool fabric which is crisp and firm to the touch will fecl'soft and compliant when severely crushed in the hand. Among the natural fibers this dualistic behavior is found only in wool and other animal hairs (not in silk, cotton, etc.), and this is one of the most attractive and valuable characteristics of wool.
  • the following examples are illustrative of this invention and are not to be construed as limitative.
  • the bircfringence (or double refraction) of the filaments was measured by the retardation technique described in Modern Textile Microscopy by J. M. Preston (London, 1933) page 270, using a petrographic microscope (Baus'ch & Lomb, Model LB) together with a 'Bausch & Lomb styleB cap analyzer compensator.
  • EXAMPLE 1 Polyethylene terephthalate in chip form having an intrinsic viscosity of 0.60 was melted on a heated grid and metered through a suitable filter pack. It was then extruded through a spinneret having fiftythree-holes into room temperature air. The extruded filaments were cooled and solidified by passage through the air and subjected after solidification to a means for winding them into a suitable package at the rate of 1206 yards per minute. The filaments of this '460 denier yarn exhibited a birefringence of 0.0060. v 7
  • the tow was then dropped in a free-toshrink condition onto an endless belt which carried it through an air oven heated to 155-165 C., the period of travel through-the oven being two minutes.
  • the resulting relaxed product, before or after cutting into staple possessed the properties shown in the following table:
  • the filaments exhibit a birefringence above 0.011, they cannot be drawn 2.7 to 4.1 times at 35-50 C., and the desired resilient product is not obtained with lower draw ratios. While they can be drawn at higher temperatures, the initial modulus of the drawn product is then considerably higher than that of fine wool.
  • the birefringence of the polyethylene terephthalate as-spun filaments is. dependent upon the polymer-intrinsic viscosity, the spinning speed and the rate of cooling of the freshly spun filaments. All other conditions being equal, an increase in the polymer intrinsic viscosity results.in a corresponding increase in the birefringence exhibited by the filaments.
  • the birefringence also increases with spinning speed as measured at the take-up and with more rapid cooling of the filaments as they leave the spinneret. This is illustrated to some extent in Example 4, where the heavier denier filaments, which do not cool as fast as the finer denier filaments, exhibits a lower birefringence.
  • the polyethylene terephthalate multi-filament yarn used in the process of this invention for the preparation of textile denier filament yarn and staple is readilyprepared by spinning 0.50 to 0.70 intrinsic viscosity polymer at speeds in the range of about 900 to 1800 yards per minute.
  • higher viscosity polymer can be used at lower spinning speeds, but such a process is not as economical.
  • lower intrinsic viscosity polymers can be spun at higher speeds to obtain the proper birefringence.
  • the spinning of the lower molecular weight polymers is more difiicult and .the tensile properties of the yarn are not so good as those of the higher intrinsic viscosity polymer yarn.
  • the polyethylene terephthalate yarn spun in the preferred manner differs from that described in the prior art, in that it can be stored indefinitely before drawing without becoming brittle and diflicult to process.
  • the yarn should be drawn to at least of its maxi- ..mum extensibility at 35 to 50 C., a draw ratio of nearly 4.1 times generally being obtained, although the ratio may be as low as 2.7 times with some yarns of the class described, particularly those whose birefringence is at or near 0.011.
  • the desired draw ratio is difiicult to obtain and the physical properties'of the final yarn are below the desired level.
  • the maximum draw ratio rapidly increases and yarn drawn to 90%-100% of the maximum extensibility will not possess the resilient properties of fine wool. If the yarn is only partially .drawn to a draw ratio of 4 at temperatures above 50 C both denier and dyeing non-uniformity result.
  • the yarn should be wet thoroughly before passing over the draw rolls. Any hydroxylated non-solvent may be .used, such as water, ethylene glycol, glycerol, and the like. Water and dilute aqueous solutions containing a finish for the yarn are preferred. As illustrated in Example 1, it is quite convenient to apply the yarn finish at this point in the process. conventional means.
  • the yarn may be wet by any drawing represents a convenient method for wetting and drawing the yarn.
  • the tray 13 contains wetting liquor heated to a temperature of around 40 C.
  • the yarn 14 to be drawn is fed over rolls 1, 2, 3 and 4, passes through the liquid bath, and is then fed over rolls 5 through 12, respectively.
  • Rolls 5, 6, 7 and 8 are 7 heated to the same temperature as thebath. The remainder of the rolls are not heated.
  • Rolls 1 through 8 arerotated at the sameperipheral speed while rolls 9 through 12 have a peripheral speed of 2.7 to 4.1 times greater. Neglecting slippage on the rolls, a drawing of 2.7 to 4.1 times takes place between rolls 8 and 9.
  • the drawing process is applicable to single ends of yarn, to a plurality .of yarn ends in warp form, or to heavy denier tows. At the low temperatures involved, heating the yarn uniformly is no problem. Equipment can, therefore, be simple and operational difficulties minivrnized.
  • the fibers and yarn prepared in accordance with this invention are capable of some spontaneous crimping when relaxed, as by being heated to an elevated temperature under little or no tension, it is preferred to crimp them mechanically. This can be accomplished conveniently by passing a tow comprising several ends of yarn through a stuffing box type crimper.
  • the crimping operation is not essential in providing the final yarn with the resilience properties of fine wool, but it aids in subsequent'mill processing. If the yarn is to be mechanically crimped, this operation is performed preferably after drawing and before relaxation.
  • the yarns are relaxed and set by heating them to temperatures in the range of 90 to 200 C. under little or no tension.
  • Suitable heating media include hot air, hot or boiling water, saturated or super-heated steam and various hot solutions th'atexert a mild plasticizing action on the material, for example, dilute nitric acid. At the higher temperatures,
  • the treatment may be for short periods of time, such as two minutes. Treatment 'at the lower temperatures should generally be for longer periods of time ranging up to 15 minutes or more, although exposure of the fibers to a shower of water at 90 -l00 C. for a few seconds has been used successfully.
  • This heat treatment stabilizes the yarn and increasesthe degree of crystallization, and also reduces residual shrinkage at the same time.
  • the fibers may be for- -warded directly from the drawing operation, or after crimping, through a suitable bath or heated chambers before being wound up or cut into staple.
  • textile-denier filaments of polyethylene terephthalate could not be drawn at temperatures below 60 C. without excessive breakage, even when wet.
  • Theas-spun yarn was 'known to become brittle on standing, and subsequent drawing of the brittle yarn-was diificult evenat'temperatures above 60 C.
  • the discovery that filaments of polyethylene terephthalate having a birefringence of 0.004 to 0.011 can be drawn wet at temperatures below 60 C. is essential to this process for preparing a synthetic fiber possessing the desirable characteristics of fine wool. Since these filaments do not become brittle on standing, an added advantage is that the as spun yarn does not have to be drawn soon after spinning.
  • An'outstanding feature of this invention is the production of a uniformly drawn product.
  • the process provides for a means of obtaining a low draw ratio while drawing the yarn to at least 90% of its maximum extensibility. That good denier uniformityis obtained is con- .firm'ed by the uniformity of subsequently dyed fabrics.
  • Another important advantage obtained from drawing the fabric may be produced from them which is crisp and firm to the touch and, nevertheless, feels soft and compliant when severely crushed in the hand.
  • These fibers and yarns of'polyethylene terephthalate materials possess, in addition, much greater strength and wearresistance thanwool fibers and arenot attacked by moths,
  • Fabrics made from these fibers are extremely lively and wrinkle resistant, with desirable drape and; excellent crease retentivity. They are remarkably insensitive to water and changes in humidity. Also of importance is the versatility which the fibers possess over and above that of wool for processing into fabrics. They are useful, particularly in staple form, in felts of variou's'kinds, including paper-makers felts, carpets, mens and womens suits, bathing suits, sweaters, knitting yarns, as the wai'p in Turkish towels and the like.
  • Suiting fabrics prepared from the staple fibers produced in accordance with this invention are particularly outstanding. These are equal to' or better than high grade woolen suiting fabrics in wrinkle resistance, :recovery from wrinkling, and retention of ironed creases. Trousers may be cleaned by washing in an'automatic washer and hanging them up todry; they do not shrink appreciably, retain their original creases, and need 'no further pressing. Y
  • a process for producing uniform artificial fibers having'the resilience characteristics of thebetter grades of wool which comprises wetting with water polyethylene terephthalate fibers of textile denier having a birefringence in the range of 0.004 to 0.011 and a corresponding maximum draw ratio of 4.1- to 2.7 at 35 -to'50? 'C., drawing the wet fibers at temperatures in the range of 35 to50 C. to at least 90% of said maximu'm'j' draw ratio, and heating'the drawn fibers in a'free-to-shrink condition at temperatures in the rangeof 90 to 200 C. until wool-like fibers are produced and relaxed and set.
  • a process for producing uniform artificial fibers having the resilience characteristics of the better-:g'rades of wool which comprises preparing polyethylene .terephthalate fibers ofxtextile denierexhibiting' birefringence in the range of 0.004 to 0.011 by spinning 0.50 to 0.70 intrinsic viscosity polymer at speeds in the range of about 900 to 1800 yards per minute, wetting the fibers with water, drawing the wet fibers at temperatures in the range of 35 to 50 C. to a maximum draw ratio of 2.7 to 4.1 times, and heating the drawn fibers in a free-toshrink condition at temperatures in the range of 90 to 200 C. until relaxed and set and characterized by woollike resilience.

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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)
  • Artificial Filaments (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
US2734794D 1951-07-12 G cm-ton Expired - Lifetime US2734794A (en)

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Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2918346A (en) * 1956-08-07 1959-12-22 Du Pont Process of orienting a dense tow of polymeric ester filaments by two step hot aqueous bath treatments
US2917779A (en) * 1955-05-13 1959-12-22 Hoechst Ag Process for preparing improved thin shaped structures, such as filaments or foils, from linear polyesters
US2931068A (en) * 1957-03-27 1960-04-05 Du Pont Process for elongating a synthetic resin structure
US2934400A (en) * 1955-03-19 1960-04-26 Glanzstoff Ag Process of manufacturing fibers of polyethylene terephthalate
US2948583A (en) * 1958-03-04 1960-08-09 Du Pont Process for producing shaped oriented polyester articles having a metallic luster
US2952078A (en) * 1953-11-30 1960-09-13 Cyril A Litzler Apparatus for controlled heating and cooling of continuous textile material
US2980492A (en) * 1958-05-27 1961-04-18 Du Pont Process for preparing textile yarns
US3091510A (en) * 1962-03-16 1963-05-28 Du Pont Process of preparing linear terephthalate polyester structures
US3097415A (en) * 1959-02-20 1963-07-16 Acrylonitrile fiber and process for
US3104450A (en) * 1958-01-08 1963-09-24 Du Pont Textile material
US3247300A (en) * 1962-10-25 1966-04-19 Du Pont Process for producing highly crimped fibers having modified surfaces
US3259681A (en) * 1962-04-27 1966-07-05 Ici Ltd Polyester filaments
US3275732A (en) * 1963-07-05 1966-09-27 Fiber Industries Inc Process for preparing thick and thin novelty yarns
US3396446A (en) * 1955-05-31 1968-08-13 Ici Ltd Process for reducing pilling in textile articles
US3415918A (en) * 1964-06-11 1968-12-10 James R. Holton Manufacture of novelty nub yarns
US3527862A (en) * 1964-02-05 1970-09-08 Teijin Ltd Process for the manufacture of polyester synthetic fibers
US3894135A (en) * 1971-10-06 1975-07-08 Zimmer Ag Process for stretching a cable of polyester threads
US4082731A (en) * 1973-02-12 1978-04-04 Avtex Fibers Inc. Method for producing a high modulus polyester yarn
US5070185A (en) * 1987-12-22 1991-12-03 Basf Corporation High shrinkage polyester fibers and method of preparation
US5139725A (en) * 1982-12-17 1992-08-18 Rhone-Poulenc Viscosuisse S.A. Process for manufacture of crimped polyester yarn from cold drawn polyester-poy yarn
KR20240109390A (ko) * 2023-01-04 2024-07-11 마남열 낚싯줄 습식 연신 장치

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2856636A (en) * 1954-12-09 1958-10-21 Eastman Kodak Co Process of treating shaped articles from non-heat-setting sulfone acid-diol polymers
IT555778A (is") * 1955-06-30
US2956308A (en) * 1958-05-21 1960-10-18 Eastman Kodak Co Chemical treatment of shaped polymeric articles

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2199411A (en) * 1938-11-01 1940-05-07 Du Pont Artificial structure and method for producing same
US2249756A (en) * 1938-10-05 1941-07-22 Du Pont Process
US2285522A (en) * 1940-05-16 1942-06-09 Fred F Lawrenz Plant support
GB603840A (en) * 1946-05-22 1948-06-23 Leslie Leben Improvements in or relating to artificial filaments, films and similar articles

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2249756A (en) * 1938-10-05 1941-07-22 Du Pont Process
US2199411A (en) * 1938-11-01 1940-05-07 Du Pont Artificial structure and method for producing same
US2285522A (en) * 1940-05-16 1942-06-09 Fred F Lawrenz Plant support
GB603840A (en) * 1946-05-22 1948-06-23 Leslie Leben Improvements in or relating to artificial filaments, films and similar articles

Cited By (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2952078A (en) * 1953-11-30 1960-09-13 Cyril A Litzler Apparatus for controlled heating and cooling of continuous textile material
US2934400A (en) * 1955-03-19 1960-04-26 Glanzstoff Ag Process of manufacturing fibers of polyethylene terephthalate
US2917779A (en) * 1955-05-13 1959-12-22 Hoechst Ag Process for preparing improved thin shaped structures, such as filaments or foils, from linear polyesters
US3396446A (en) * 1955-05-31 1968-08-13 Ici Ltd Process for reducing pilling in textile articles
US2918346A (en) * 1956-08-07 1959-12-22 Du Pont Process of orienting a dense tow of polymeric ester filaments by two step hot aqueous bath treatments
US2931068A (en) * 1957-03-27 1960-04-05 Du Pont Process for elongating a synthetic resin structure
US2952879A (en) * 1957-03-27 1960-09-20 Du Pont Process of preparing spontaneously extensible structures
US3104450A (en) * 1958-01-08 1963-09-24 Du Pont Textile material
US2948583A (en) * 1958-03-04 1960-08-09 Du Pont Process for producing shaped oriented polyester articles having a metallic luster
US2980492A (en) * 1958-05-27 1961-04-18 Du Pont Process for preparing textile yarns
US3097415A (en) * 1959-02-20 1963-07-16 Acrylonitrile fiber and process for
US3091510A (en) * 1962-03-16 1963-05-28 Du Pont Process of preparing linear terephthalate polyester structures
US3259681A (en) * 1962-04-27 1966-07-05 Ici Ltd Polyester filaments
US3247300A (en) * 1962-10-25 1966-04-19 Du Pont Process for producing highly crimped fibers having modified surfaces
US3275732A (en) * 1963-07-05 1966-09-27 Fiber Industries Inc Process for preparing thick and thin novelty yarns
US3527862A (en) * 1964-02-05 1970-09-08 Teijin Ltd Process for the manufacture of polyester synthetic fibers
US3415918A (en) * 1964-06-11 1968-12-10 James R. Holton Manufacture of novelty nub yarns
US3894135A (en) * 1971-10-06 1975-07-08 Zimmer Ag Process for stretching a cable of polyester threads
US4082731A (en) * 1973-02-12 1978-04-04 Avtex Fibers Inc. Method for producing a high modulus polyester yarn
US5139725A (en) * 1982-12-17 1992-08-18 Rhone-Poulenc Viscosuisse S.A. Process for manufacture of crimped polyester yarn from cold drawn polyester-poy yarn
US5070185A (en) * 1987-12-22 1991-12-03 Basf Corporation High shrinkage polyester fibers and method of preparation
KR20240109390A (ko) * 2023-01-04 2024-07-11 마남열 낚싯줄 습식 연신 장치
KR102754550B1 (ko) 2023-01-04 2025-01-13 마남열 낚싯줄 습식 연신 장치

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FR1066203A (fr) 1954-06-03
GB721912A (en) 1955-01-12

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