EP3814562A1 - Filé comprenant une fibre discontinue de polyester et tissu le comprenant - Google Patents

Filé comprenant une fibre discontinue de polyester et tissu le comprenant

Info

Publication number
EP3814562A1
EP3814562A1 EP19746554.5A EP19746554A EP3814562A1 EP 3814562 A1 EP3814562 A1 EP 3814562A1 EP 19746554 A EP19746554 A EP 19746554A EP 3814562 A1 EP3814562 A1 EP 3814562A1
Authority
EP
European Patent Office
Prior art keywords
fabric
staple fiber
spun
spun yarn
pet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP19746554.5A
Other languages
German (de)
English (en)
Inventor
Steven R. ACKERMAN
Akshay Kumar
Dennis Gerard Madeleine
Wayne E. Marsh
Kalika Ranjan Samant
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Covation Inc
Original Assignee
DuPont Industrial Biosciences USA LLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by DuPont Industrial Biosciences USA LLC filed Critical DuPont Industrial Biosciences USA LLC
Publication of EP3814562A1 publication Critical patent/EP3814562A1/fr
Pending legal-status Critical Current

Links

Classifications

    • 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
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • 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
    • D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
    • 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • 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
    • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
    • D02G3/04—Blended or other yarns or threads containing components made from different materials
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]

Definitions

  • the present disclosure is directed towards spun yarn comprising melt spun staple fiber comprising a first polymer and a second polymer, and to fabrics comprising the spun yarn.
  • the first polymer comprises poly(trimethylene terephthalate) or poly(butylene terephthalate)
  • the second polymer comprises poly(ethylene terephthalate) or Co-PET, wherein Co-PET is a polyethylene terephthalate) copolymer comprising isophthalic acid monomer.
  • Poly(trimethylene terephthalate) is a commercial fiber, offering desirable properties such as easy disperse dyeability at atmospheric pressure, relatively low bending modulus, and relatively high elastic recovery and
  • Shrinkage is affected by storage time and storage temperature, and uncontrolled shrinkage leads to denier nonuniformity and draw breaks during the drawing process. As a result, commercialization of PTT staple or blends of PTT staple with natural fibers has been limited.
  • staple fibers are preferred over continuous filament.
  • staple spun yarns for apparel fabrics require
  • Staple fibers additionally allow blending synthetic fibers with natural fibers, such as wool, cotton, and cellulose.
  • the manufacture of staple fiber suitable for fabrics can present special problems, particularly in conventional split spin/draw processes where the drawing is carried out in a separate step and characteristics of the undrawn fiber, for example dry heat shrinkage, can change as the undrawn fiber ages during storage.
  • PTT-based staple of good uniformity and tenacity, and economical processes to produce such staple.
  • spun yarns comprising PTT-based staple fiber and having good tenacity and elongation at break, and which can impart desired qualities to fabrics comprising such spun yarns.
  • melt spun staple fibers spun yarns comprising the melt spun staple fibers, and fabrics comprising the spun yarns.
  • spun yarn comprising melt spun staple fiber comprising a first polymer comprising poly(trimethylene
  • the first polymer comprises poly(trimethylene terephthalate) and the weight ratio of the poly(trimethylene terephthalate) to the second polymer is in the range of from about 80:20 to about 10:90; or the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90.
  • the weight ratio of the poly(trimethylene terephthalate) or the poly(butylene terephthalate) to the second polymer is in the range of from about 70:30 to 30:70.
  • the spun yarn has a boil off shrinkage of at least about 6% as determined according to ASTM D2259.
  • the melt spun staple fiber comprises poly(trimethylene terephthalate) and poly(ethylene terephthalate). In another embodiment of the spun yarn, the melt spun staple fiber comprises poly(trimethylene terephthalate) and Co-PET. In one embodiment of the spun yarn, the first polymer comprises poly(trimethylene terephthalate) and the second polymer comprises Co-PET, and the co-PET contains from about 0.5 mole percent to about 10 mole percent isophthalic acid monomer, based on the total copolymer composition. In an additional embodiment of the spun yarn, the melt spun staple fiber comprises poly(butylene terephthalate) and poly(ethylene terephthalate).
  • the melt spun staple fiber comprises poly(butylene terephthalate) and Co-PET.
  • the first polymer comprises poly(butylene terephthalate) and the second polymer comprises Co-PET, and the Co-PET contains from about 0.5 mole percent to about 10 mole percent isophthalic acid monomer, based on the total copolymer composition.
  • the second polymer comprises Co-PET, and the Co-PET contains from about 0.5 mole percent to about 10 mole percent isophthalic acid monomer, based on the total copolymer composition.
  • the spun yarn further comprises a second staple fiber in an amount from about 5 wt% to about 95 wt%, based on the total weight of the spun yarn.
  • the second staple fiber comprises polylactic acid, acrylic, nylon, olefin, acetate, rayon, or polyester.
  • the second staple fiber comprises at least one natural fiber selected from cotton, linen, wool, angora, mohair, alpaca, or cashmere.
  • the second staple fiber comprises polylactic acid, acrylic, nylon, olefin, acetate, rayon, polyester, cotton, linen, wool, angora, mohair, alpaca, cashmere, or a mixture thereof.
  • the second staple fiber comprises cotton or wool.
  • the second staple fiber comprises cotton.
  • the spun yarn further comprises a second staple fiber comprising cotton, and the cotton is present in an amount from about 5 wt% to about 95 wt%, based on the total weight of the spun yarn.
  • the spun yarn further comprising cotton has a cotton count of about 4 Ne to about 80 Ne.
  • the second staple fiber comprises wool.
  • the spun yarn further comprises a second staple fiber comprising wool, and the wool is present in an amount from about 5 wt% to about 95 wt%, based on the total weight of the spun yarn.
  • the spun yarn further comprising wool has a worsted count in the range of from 7 Nm to 120 Nm.
  • a fabric comprising a spun yarn as disclosed herein.
  • the fabric has a softer hand and better drape than a fabric of the same fabric construction consisting of rayon, polyethylene terephthalate, cotton, or a combination thereof.
  • the fabric has at least one of: i) better abrasion resistance as determined according to ASTM D4966 Standard Test Method; ii) higher pill rating values as determined according to ASTM D4970 Standard Test Method,; or iii) greater bulk as determined according to ASTM D1777 Standard Test Method; than a fabric of the same fabric construction consisting of polyethylene
  • the fabric has better dyeability than a fabric of the same construction consisting of polyethylene terephthalate, cotton, rayon, or a combination thereof.
  • the fabric has better abrasion resistance than a fabric of the same fabric construction consisting of polyethylene terephthalate, cotton, rayon, or a combination thereof.
  • the fabric has less pilling (higher pill rating values) than a fabric of the same fabric construction consisting of polyethylene terephthalate, cotton, rayon, or a combination thereof.
  • the fabric has greater bulk than a fabric of the same fabric construction consisting of polyethylene terephthalate, cotton, rayon, or a combination thereof.
  • the fabric is a woven fabric having a warp and a weft.
  • the fabric is a woven fabric having a warp and a weft, and the warp, the weft, or both the warp and the weft each comprise a spun yarn as disclosed herein.
  • the warp comprises a spun yarn as disclosed herein.
  • the weft comprises a spun yarn as disclosed herein.
  • the warp and the weft each comprise a spun yarn as disclosed herein.
  • the fabric is a knit fabric.
  • the knit fabric has higher recovery than a knit fabric of the same fabric construction consisting of polyethylene terephthalate, cotton, rayon, or a combination thereof.
  • articles comprising a fabric as disclosed herein, for example a garment.
  • melt spun staple fiber comprising a first polymer comprising poly(trimethylene terephthalate) or poly(butylene terephthalate) and a second polymer comprising polyethylene terephthalate) or Co-PET, wherein Co-PET is a poly(ethylene terephthalate) copolymer comprising isophthalic acid monomer, the staple fiber having a weight ratio of the first polymer to the second polymer in the range of about 70:30 to about 30:70, and a dry heat shrinkage of less than 6% as determined by the Dry Heat Shrinkage Method.
  • the melt spun staple fiber comprises poly(trimethylene terephthalate) and polyethylene terephthalate).
  • the melt spun staple fiber comprises poly(trimethylene terephthalate) and Co-PET.
  • the melt spun staple fiber comprises poly(butylene terephthalate) and polyethylene terephthalate).
  • the melt spun staple fiber comprises poly(butylene terephthalate) and Co-PET
  • the second polymer comprises Co-PET, and the Co-PET contains from about 0.5 mole percent to about 10 mole percent isophthalic acid monomer, based on the total copolymer composition.
  • the weight ratio of the first polymer to the second polymer is in the range of from about 70:30 to 50:50.
  • the term“about” refers to a range of +/- 0.5 of the numerical value, unless the term is otherwise specifically defined in context.
  • the phrase a“pH value of about 6” refers to pH values of from 5.5 to 6.5, unless the pH value is specifically defined otherwise.
  • poly(trimethylene terephthalate) or PTT is meant polymer comprising repeat units derived from 1 ,3-propanediol and terephthalic acid (or equivalent).
  • poly(trimethylene terephthalate) homopolymer means polymer of substantially only 1 ,3-propanediol and terephthalic acid (or
  • poly(trimethylene terephthalate) also includes PTT copolymers, by which is meant polymer comprising repeat units derived from 1 ,3-propanediol and terephthalic acid (or equivalent) and also containing at least one additional unit derived from an additional monomer.
  • PTT copolymers examples include copolyesters made using 3 or more reactants, each having two ester forming groups. For example, a
  • copoly(trimethylene terephthalate) can be used in which the comonomer used to make the copolyester is selected from the group consisting of linear, cyclic, and branched aliphatic dicarboxylic acids having 4-12 carbon atoms (for example butanedioic acid, pentanedioic acid, hexanedioic acid, dodecanedioic acid, and 1 ,4-cyclo-hexanedicarboxylic acid); aromatic dicarboxylic acids other than terephthalic acid and having 8-12 carbon atoms (for example isophthalic acid and 2,6-naphthalenedicarboxylic acid); linear, cyclic, and branched aliphatic diols having 2-8 carbon atoms (other than 1 ,3-propanediol, for example, ethanediol, 1 ,2-propanediol, 1 ,4-butanediol
  • the term“poly(butylene terephthalate)” or PBT means polymer derived from substantially only 1 ,4-butanediol and terephthalic acid, and is also referred to as poly(butylene terephthalate) homopolymer.
  • the term“poly(butylene terephthalate) copolymer refers to polymer comprising repeat units derived from 1 ,4-butanediol and terephthalic acid and also
  • poly(ethylene terephthalate) or PET means polymer derived from substantially only ethylene glycol and terephthalic acid (or equivalent, such as dimethyl terephthalate), and is also referred to as
  • polyethylene terephthalate polyethylene terephthalate homopolymer
  • poly(ethylene terephthalate) copolymer refers to polymer comprising repeat units derived from ethylene glycol and terephthalic acid (or equivalent) and also containing at least one additional unit derived from an additional monomer.
  • Co-PET refers to poly(ethylene terephthalate) copolymers in which the additional monomer is isophthalic acid (or an ester equivalent).
  • Co-PET is a poly(ethylene terephthalate) copolymer comprising ethylene terephthalate and isophthalic acid monomers.
  • “Staple” refers to either natural fibers or cut lengths from filaments.
  • the term staple (fiber) is used in the textile industry to distinguish natural or cut man- made fibers from filament.
  • Man-made fibers are cut to a specific length, for example, as long as 8 inches or as short as 1.5 inches or less, so they can be processed on cotton, woolen, or worsted yarn spinning systems, or flocked.
  • melt spun staple fiber refers to staple fiber obtained by melting a fiber-forming substance, extruding it through a spinneret, then solidifying it directly by cooling; such melt spun fiber is stored, combined with other batches of melt spun fiber obtained similarly, and collectively drawn, crimped, heat treated for stabilization, and cut to obtain staple fiber.
  • spun yarn refers to yarn produced by aligning cut staple fibers in multiple steps wherein a tow of cut staple fibers is successively drafted into a lower and lower denier continuous strand and in which the staple fibers are bound together by twist.
  • Undrawn yarn is a term customarily applied to fiber that has not been drawn, and is not intended herein to include fibers that have been drawn and processed into a yarn product, such as those yarns used in knitting or weaving fabric. After melt spinning, undrawn yarn is accumulated until an appropriate total denier for the draw machine is produced. Accumulation can take up to 24 hours or more including dormant or storage time between steps. For example, making sufficient undrawn yarn for economic drawing at the draw line generally takes 6 hours or more. Due to production scheduling and other practical considerations, fiber may be stored for several days. Fiber having been exposed to such storage time is referred to as“aged” or“aged undrawn yarn”.
  • “Draw ratio”, or“draw down”, is the amount by which filaments are stretched following melt spinning.
  • “draw ratio” refers to machine draw ratio, which is the ratio of the surface speed of the pulling rolls to the forwarding rolls (rolls that move the fiber). As a result of pulling, some stretching occurs.
  • “Carding” is a process whereby staple fiber bunch is opened,
  • the card machine consists of a series of rolls whose surfaces are covered with many projecting metal teeth or pins.
  • Tow means a large strand of continuous manufactured fiber filaments without definite twist, collected in loose, rope-like form before being cut into staple or formed into sliver.
  • A“sliver” is a continuous strand of loosely assembled staple fibers without twist. Sliver is delivered by the card or drawing frame. The production of sliver is the first step in the textile operation that converts staple fiber into a form that can be drawn and eventually twisted into a spun yarn.
  • fabric means a planar textile structure produced by interlacing yarns, fibers, or filaments.
  • woven fabric means a fabric composed of warp yarns and filling (weft) yarns which are interlaced.
  • weft filling
  • the lengthwise or longitudinal warp yarns are held stationary in tension on a frame or loom while the transverse weft (which can also be referred to as woof) is drawn through and inserted over-and-under the warp.
  • the term“knit fabric” means a fabric produced by interlooping one or more ends of yarn.
  • fabric construction means the details of the structure of a fabric, including the style, width, type of weave or knit, number of yarns per inch in the warp and weft, and the weight of goods.
  • decitex is a unit of measure for the linear mass density of fiber or yarn, and is defined as the mass in grams per 10,000 meters.
  • sliver linear density means the weight in grams of a one meter length of sliver.
  • sliver linear density means the number of 840 yards cut length of sliver in one pound weight, expressed in English count Ne, or weight of sliver in grams in 1000 meter length expressed as g/meter.
  • final sliver linear density means the number of 840 yards cut length of sliver in one pound weight expressed in English count Ne, or weight of sliver in grams in one meter expressed as g/meter.
  • unevenness % means the average mean deviation in weight of a 400 meter length of spun yarn, or in a 50 meter length of roving or a 50 meter length of sliver, as measured by Uster evenness tester-3 (UT3), expressed as a percentage. Measured by industrial established method using UT-3 and 400 m length of yarn or 25 m or 50 m length of sliver or roving.
  • the term“imperfections” with regard to spun yarn means the numerical sum of the number of thick regions, the number of thin regions, and the number of neps in a 1000 meter length of yarn, as determined using a Uster evenness tester.
  • the term“thick region” means a place on the spun yarn having mass greater than or equal to +150% of the average mass of the yarn in a 8 mm cut length.
  • the term“thin region” means a place on the spun yarn having mass less than or equal to 50% of average mass of the yarn in a 8 mm cut length.
  • the term“neps” means a place on the spun yarn having mass greater than or equal to 200% of the average mass of the yarn in a 1 mm cut length.
  • hairiness index refers to the average of total length of protruding fiber per 1 cm length of yarn measured in 400 m length of yarn, measured optically using a UT3 tester, expressed as normalized units.
  • the present disclosure is directed to spun yarn comprising melt spun staple fiber comprising a first polymer comprising poly(trimethylene
  • the first polymer comprises poly(trimethylene terephthalate) and the weight ratio of the poly(trimethylene terephthalate) to the second polymer is in the range of about 80:20 to about 10:90; or the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90.
  • the melt spun staple fiber lacks any distinct interface between the first and second polymers.
  • the spun yarn has a boil off shrinkage of at least about 6%, as determined according to ASTM D2259.
  • the spun yarn can comprise a second staple fiber, for example cotton or wool. Fabrics with desirable characteristics can be made from the spun yarns.
  • melt spun staple fiber disclosed herein has improved tenacity, crimp, and stability in comparison to PTT melt spun staple fiber, and the properties of the melt spun staple fiber advantageously enable processing under conditions typically used with PET during staple conversion into spun yarns. Additionally, the spun yarns comprising the melt spun staple fiber disclosed herein, whether further comprising a second staple fiber or consisting essentially of the melt spun staple fiber alone, enable production of woven, knitted, and nonwoven fabrics having cotton-like aesthetics, good strength, and other desirable attributes.
  • the melt spun staple fiber of the spun yarn comprises a first polymer comprising poly(trimethylene terephthalate).
  • Poly(trimethylene terephthalate) suitable for use in the melt spun staple fiber is well known in the art and can be prepared, for example, by polycondensation of 1 ,3-propane diol with terephthalic acid or terephthalic acid equivalent.
  • the 1 ,3-propane diol may be obtained biochemically from a renewable source (“biologically- derived” 1 ,3-propanediol).
  • Poly(trimethylene terephthalate)s are commercially available from E. I. du Pont de Nemours and Company, Wilmington, DE under the trademark Sorona®.
  • PTT or its monomers could be obtained from recycling post-industrial or post-consumer materials (i.e. fiber or plastic waste).
  • terephthalic acid equivalent is meant compounds that perform substantially like terephthalic acids in reaction with polymeric glycols and diols, as would be generally recognized by a person of ordinary skill in the relevant art.
  • Terephthalic acid equivalents include, for example, esters (such as dimethyl terephthalate), and ester-forming derivatives such as acid halides (e.g., acid chlorides) and anhydrides.
  • esters such as dimethyl terephthalate
  • ester-forming derivatives such as acid halides (e.g., acid chlorides) and anhydrides.
  • acid halides e.g., acid chlorides
  • anhydrides e.g., acid chlorides
  • poly(trimethylene terephthalate) are disclosed, for example, in US6277947, US6326456, US6657044, US6353062, US6538076, and US7531617.
  • the 1 ,3-propanediol used as a reactant or as a component of the reactant in making poly(trimethylene terephthalate) has a purity of greater than about 99%, for example greater than about 99.9%, by weight as determined by gas chromatographic analysis.
  • Purified 1 ,3-propanediols are disclosed in US7038092, US7098368, US7084311 , and US7919658.
  • Poly(trimethylene terephthalate) suitable for use in the melt spun fibers can be poly(trimethylene terephthalate) homopolymers (derived substantially from 1 ,3-propane diol and terephthalic acid and/or equivalent) and copolymers.
  • the poly(trimethylene terephthalate) contains about 70 mole % or more of repeat units derived from 1 ,3-propane diol and terephthalic acid (and/or an equivalent thereof, such as dimethyl terephthalate).
  • poly(trimethylene terephthalate) can contain at least about 85 mole %, or at least about 90 mole %, or at least about 95 mole %, or at least about 99 mole %, or about 100 mole% of repeat units derived from 1 ,3-propane diol and terephthalic acid (or equivalent).
  • the poly(trimethylene terephthalate) can contain minor amounts of other comonomers, and such comonomers are usually selected so that they do not have a significant adverse effect on properties.
  • Such other comonomers include 5-sodium-sulfoisophthalate, for example, at a level in the range of about 0.2 to 5 mole %.
  • Very small amounts of trifunctional comonomers, for example trimellitic acid, can be incorporated for viscosity control.
  • the poly(trimethylene terephthalate) can contain up to 30 mole % of repeat units made from other diols or diacids.
  • Other diacids include, for example, isophthalic acid, 1 ,4-cyclohexane dicarboxylic acid, 2,6-naphthalene dicarboxylic acid, 1 ,3-cyclohexane dicarboxylic acid, succinic acid, glutaric acid, adipic acid, sebacic acid, 1 ,12-dodecane dioic acid, and the derivatives thereof such as the dimethyl, diethyl, or dipropyl esters of these dicarboxylic acids.
  • diols include ethylene glycol, 1 ,4-butane diol, 1 ,2-propanediol, diethylene glycol, triethylene glycol, 1 ,3-butane diol, 1 ,5-pentane diol, 1 ,6-hexane diol, 1 ,2- 1 ,3- and 1 ,4-cyclohexane dimethanol, and the longer chain diols and polyols made by the reaction product of diols or polyols with alkylene oxides.
  • the poly(trimethylene terephthalate) can also include functional monomers, for example, up to about 5 mole % of sulfonate compounds useful for imparting cationic dyeability. Specific examples of preferred sulfonate
  • compounds include 5-lithium sulfoisophthalate, 5-sodium sulfoisophthalate, 5- potassium sulfoisophthalate, 4-sodium sulfo-2,6-naphthalenedicarboxylate, tetramethylphosphonium 3,5-dicarboxybenzene sulfonate,
  • Poly(trimethylene terephthalate) has an intrinsic viscosity that typically is about 0.5 deciliters/gram (dl/g) or higher, and typically is about 2 dl/g or less.
  • the poly(trimethylene terephthalate) has an intrinsic viscosity that is about 0.7 dl/g or higher, for example 0.8 dl/g or higher, or for example 0.9 dl/g or higher, and typically it is about 1.5 dl/g or less, for example 1.4 dl/g or less, and commercial products presently available have intrinsic viscosities of 1.2 dl/g or less.
  • the melt spun staple fiber of the spun yarn comprises a first polymer comprising poly(butylene terephthalate).
  • Poly(butylene terephthalate) suitable for use in the melt spun staple fiber is also well known in the art and can be prepared, for example, by polycondensation of 1 ,4-butanediol with terephthalic acid.
  • Poly(butylene terephthalate)s are commercially available from E. I. du Pont de Nemours and Company, Wilmington, DE under the trademark Crastin®.
  • Poly(butylene terephthalate) suitable for use in the melt spun fibers can be homopolymers (derived substantially from 1 ,4-butanediol and terephthalic acid and/or equivalent) and copolymers.
  • the poly(butylene terephthalate) contains about 80 mole % or more of repeat units derived from 1 ,4-butanediol and terephthalic acid.
  • the poly(butylene terephthalate) can contain at least about 85 mole %, or at least about 90 mole %, or at least about 95 mole %, or at least about 99 mole %, or about 100 mole% of repeat units derived from 1 ,4-butanediol and terephthalic acid (or equivalent).
  • the poly(trimethylene terephthalate) can contain minor amounts of other comonomers or functional monomers.
  • PBT or its monomers could be obtained from recycling post-industrial or post-consumer materials (i.e. fiber or plastic waste).
  • Polyethylene terephthalate is a polyester that may be prepared by the condensation polymerization of ethylene glycol and terephthalic acid (or dimethyl terephthalate or other terephthalate ester). Processes for producing polyethylene terephthalate) are known, for example as disclosed in US3398124 and US3487049. Poly(ethylene terephthalate) suitable for use in preparing the melt spun staple fiber disclosed herein is also commercially available. In one embodiment, the poly(ethylene terephthalate) is a homopolymer and is derived substantially from ethylene glycol and terephthalic acid and/or equivalent.
  • PET or its monomers could be obtained from recycling post-industrial or post-consumer material (i.e. fiber or plastic waste).
  • a copolymer of polyethylene terephthalate can be prepared from monomers of dimethyl terephthalate or terephthalic acid in combination with cyclohexane dimethanol, or in combination with cyclohexane dimethanol and ethylene glycol.
  • isophthalic acid can be used to replace a portion of the
  • “Co-PET” refers to polyethylene terephthalate) copolymers that may be prepared by the condensation polymerization of ethylene glycol, terephthalic acid (or dimethyl terephthalate or other terephthalate ester) and isophthalic acid (or dimethyl isophthalate or other terephthalate ester), as known in the art.
  • Co-PET can also be produced in a process in which recycled poly(ethylene terephthalate) bottles are chopped, melted, purified, and repelletized to produce fiber-grade post-consumer recycled Co-PET.
  • the isophthalic acid monomer is typically present in Co-PET at a level in the range of about 0.5 mole % to about 15 mole %, and can be present in amounts up to about 30 mole %, based on the total copolymer composition.
  • Co- PET can contain about 0.5, 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13, 14, 15, 16, 17,
  • Co-PET useful in the melt spun staple fibers disclosed herein contains from about 1 mole % to about 5 mole%, or up to about 10 mole%, or up to about 15 mole%, isophthalic acid monomer, based on the total copolymer composition.
  • useful Co-PET contains from about 0.5 mol % to about 3 mole% isophthalic acid monomer.
  • the amount of isophthalic acid monomer in Co-PET can be selected to provide the desired properties to the Co-PET. It is thought that the lower melting point of Co-PET can improve the compatibility of Co-PET and poly(trimethylene terephthalate) during melt spinning. Co-PET is commercially available.
  • a polyethylene terephthalate copolymer containing an additional monomer other than isophthalic acid may be used.
  • a polyethylene terephthalate copolymer comprising ethylene glycol, terephthalic acid (or equivalent), and a dicarboxylic acid such as succinic acid, adipic acid, azelaic acid, sebacic acid, glutaric acid, 1 ,10-decanedicarboxylic acid, phthalic acid, dodecanedioic acid, sulfonated isophthalic acid, oxalic acid, fumaric acid, maleic acid, itaconic acid, 1 ,4-cyclohexanedicarboxylic acid, 1 ,3- cyclohexanedicarboxylic acid, 1 ,2-cyclohexanedicarboxylic acid, and mixtures there of may be useful in preparing a melt spun staple fiber.
  • a polyethylene terephthalate copolymer comprising ethylene glycol, terephthalic acid (or equivalent), and a diol such as diethylene glycol, polyethylene glycol, butylene glycol, 1 ,4-cyclohexane dimethanol, 1 ,2-cyclohexanediol, 1 ,4- cyclohexanediol, 1 ,3-cyclohexanediol, 1 ,5-pentanediol, 1 ,6-hexanediol, and mixtures thereof may be useful in preparing a melt spun staple fiber.
  • a diol such as diethylene glycol, polyethylene glycol, butylene glycol, 1 ,4-cyclohexane dimethanol, 1 ,2-cyclohexanediol, 1 ,4- cyclohexanediol, 1 ,3-cyclohexanediol, 1 ,5-p
  • Co-PET is a poly(ethylene terephthalate) copolymer comprising ethylene terephthalate and isophthalic acid monomers.
  • Co-PET is a poly(ethylene terephthalate) copolymer consisting essentially of polyethylene terephthalate) and isophthalic acid monomers.
  • Co-PET is a poly(ethylene terephthalate) copolymer consisting of poly(ethylene terephthalate) and isophthalic acid monomers.
  • the melt spun staple fiber comprises a first polymer comprising
  • the melt spun staple fiber comprises poly(trimethylene terephthalate) (PTT) and
  • the melt spun staple fiber comprises about 80 weight percent PTT and about 20 weight percent PET.
  • the melt spun staple fiber comprises about 75 weight percent PTT and about 25 weight percent PET.
  • the melt spun staple fiber comprises about 70 weight percent PTT and about 30 weight percent PET.
  • the staple fiber comprises about 65 weight percent PTT and about 35 weight percent PET.
  • the staple fiber comprises about 60 weight percent PTT and about 40 weight percent PET.
  • the staple fiber comprises about 55 weight percent PTT and about 45 weight percent PET.
  • the staple fiber comprises about 50 weight percent PTT and about 50 weight percent PET.
  • the staple fiber comprises about 45 weight percent PTT and about 55 weight percent PET.
  • the staple fiber comprises about 40 weight percent PTT and about 60 weight percent PET. In another embodiment, the staple fiber comprises about 35 weight percent PTT and about 65 weight percent PET. In yet another embodiment, the staple fiber comprises about 30 weight percent PTT and about 70 weight percent PET. In one embodiment, the melt spun staple fiber comprises about 25 weight percent PTT and about 75 weight percent PET. In one embodiment, the melt spun staple fiber comprises about 20 weight percent PTT and about 80 weight percent PET.
  • the melt spun staple fiber comprises about 15 weight percent PTT and about 85 weight percent PET. In one embodiment, the melt spun staple fiber comprises about 10 weight percent PTT and about 90 weight percent PET.
  • melt spun staple fiber comprises
  • the melt spun staple fiber comprises about 80 weight percent PTT and about 20 weight percent Co-PET. In an additional embodiment, the melt spun staple fiber comprises about 75 weight percent PTT and about 25 weight percent Co-PET. In one embodiment, the melt spun staple fiber comprises about 70 weight percent PTT and about 30 weight percent Co-PET. In another embodiment, the melt spun staple fiber comprises about 65 weight percent PTT and about 35 weight percent Co-PET.
  • the melt spun staple fiber comprises about 60 weight percent PTT and about 40 weight percent Co-PET. In an additional embodiment, the melt spun staple fiber comprises about 55 weight percent PTT and about 45 weight percent Co-PET. In a further embodiment, the melt spun staple fiber comprises about 50 weight percent PTT and about 50 weight percent Co-PET. In another embodiment, the melt spun staple fiber comprises about 45 weight percent PTT and about 55 weight percent Co-PET. In a separate embodiment, the melt spun staple fiber comprises about 40 weight percent PTT and about 60 weight percent Co-PET. In another embodiment, the melt spun staple fiber comprises about 35 weight percent PTT and about 65 weight percent Co-PET. In yet another embodiment, the melt spun staple fiber comprises about 30 weight percent PTT and about 70 weight percent Co-PET. In one embodiment, the melt spun staple fiber comprises about 25 weight percent PTT and about 75 weight percent Co-PET. In another
  • the melt spun staple fiber comprises about 20 weight percent PTT and about 80 weight percent Co-PET. In yet another embodiment, the melt spun staple fiber comprises about 15 weight percent PTT and about 85 weight percent Co-PET. In an additional embodiment, the melt spun staple fiber comprises about 10 weight percent PTT and about 90 weight percent Co-PET.
  • the melt spun staple fiber comprises poly(butylene terephthalate) (PBT) and poly(ethylene terephthalate) (PET), and the melt spun staple fiber comprises about 90 weight percent PBT and about 10 weight percent PET. In another embodiment, the melt spun staple fiber comprises about 85 weight percent PBT and about 15 weight percent PET. In one embodiment, the melt spun staple fiber comprises about 80 weight percent PBT and about 20 weight percent PET. In one embodiment, the melt spun staple fiber comprises about 75 weight percent PBT and about 25 weight percent PET. In one embodiment, the melt spun staple fiber comprises about 70 weight percent PBT and about 30 weight percent PET. In another embodiment, the staple fiber comprises about 65 weight percent PBT and about 35 weight percent PET.
  • the staple fiber comprises about 60 weight percent PBT and about 40 weight percent PET. In an additional embodiment, the staple fiber comprises about 55 weight percent PBT and about 45 weight percent PET. In a further embodiment, the staple fiber comprises about 50 weight percent PBT and about 50 weight percent PET. In another embodiment, the staple fiber comprises about 45 weight percent PBT and about 55 weight percent PET. In a separate embodiment, the staple fiber comprises about 40 weight percent PBT and about 60 weight percent PET. In another embodiment, the staple fiber comprises about 35 weight percent PBT and about 65 weight percent PET. In yet another embodiment, the staple fiber comprises about 30 weight percent PBT and about 70 weight percent PET. In one embodiment, the melt spun staple fiber comprises about 25 weight percent PBT and about 75 weight percent PET.
  • the melt spun staple fiber comprises about 20 weight percent PBT and about 80 weight percent PET. In one embodiment, the melt spun staple fiber comprises about 15 weight percent PBT and about 85 weight percent PET. In one embodiment, the melt spun staple fiber comprises about 10 weight percent PBT and about 90 weight percent PET.
  • the melt spun staple fiber comprises poly(butylene terephthalate (PBT) and a polyethylene terephthalate) copolymer comprising isophthalic acid monomer (Co-PET), and the weight ratio of PBT to Co-PET is in the range of about 90:10 to about 10:90.
  • the melt spun staple fiber comprises about 85 weight percent PBT and about 15 weight percent Co-PET.
  • the melt spun staple fiber comprises about 80 weight percent PBT and about 20 weight percent Co-PET.
  • the melt spun staple fiber comprises about 75 weight percent PBT and about 25 weight percent Co-PET.
  • the melt spun staple fiber comprises about 70 weight percent PBT and about 30 weight percent Co- PET.
  • the melt spun staple fiber comprises about 65 weight percent PBT and about 35 weight percent Co-PET. In yet another embodiment, the melt spun staple fiber comprises about 60 weight percent PBT and about 40 weight percent Co-PET. In an additional embodiment, the melt spun staple fiber comprises about 55 weight percent PBT and about 45 weight percent Co-PET. In a further embodiment, the melt spun staple fiber comprises about 50 weight percent PBT and about 50 weight percent Co-PET. In another embodiment, the melt spun staple fiber comprises about 45 weight percent PBT and about 55 weight percent Co-PET. In a separate embodiment, the melt spun staple fiber comprises about 40 weight percent PBT and about 60 weight percent Co-PET. In another embodiment, the melt spun staple fiber comprises about 35 weight percent PBT and about 65 weight percent Co-PET.
  • the melt spun staple fiber comprises about 30 weight percent PBT and about 70 weight percent Co-PET. In one embodiment, the melt spun staple fiber comprises about 25 weight percent PBT and about 75 weight percent Co- PET. In another embodiment, the melt spun staple fiber comprises about 20 weight percent PBT and about 80 weight percent Co-PET. In yet another embodiment, the melt spun staple fiber comprises about 15 weight percent PBT and about 85 weight percent Co-PET. In an additional embodiment, the melt spun staple fiber comprises about 10 weight percent PBT and about 90 weight percent Co-PET.
  • the melt spun staple fiber can be formed in a two-stage process.
  • the polymers are combined, melted, extruded to form filaments comprising the polymers, the filaments are cooled, and collected as tow.
  • the tow can be processed through at least one stage of draw, crimped, annealed, and cut to produce staple fiber. Processes to prepare polyester staple fiber are known, for example as disclosed in US 5,308,564.
  • the first polymer (PTT or PBT) and the second polymer (PET or Co-PET), can be combined by any known technique.
  • the polymers can be combined in a variety of ways, for example they can be (a) heated and mixed simultaneously,
  • the mixing, heating, and forming can be carried out by conventional equipment designed for that purpose such as extruders.
  • the temperature should be above the melting points of each polymer but below the lowest decomposition temperature. Suitable temperatures can be in the range of about 140 °C to about 240 °C, for example at least about 200 °C and up to about 230 °C. In one embodiment, the melt temperature is below 280 °C.
  • the polymers can be compounded, for example in a compounding screw, in a desired ratio to form pellets which are then fed to a spinning machine extruder.
  • pellets can be made of each polymer separately, and then the pellets are blended together as a salt-and- pepper mixture using up to two feeders to a spinning machine extruder.
  • pellets can be made of each polymer separately, and the pellets pre-mixed together before being fed to a spinning machine extruder.
  • each polymer can be melted to form a molten polymer stream, and then the molten polymer streams can be combined, and pellets formed from the molten mixture.
  • pellets is used generically herein, and is used regardless of shape so that it includes products sometimes called “chips” or“flakes”.
  • additives can be added to the poly(trimethylene terephthalate), to the poly(butylene terephthalate), to the poly(ethylene terephthalate), to the Co- PET, or to the mixture of polymers.
  • Useful additives can include, for example, delusterants, nucleating agents, heat stabilizers, viscosity boosters, optical brighteners, antioxidants, antimicrobials, plasticizers, anti-static agents, lubricants, processing aids, flame retardants, dyes, T1O2, or pigments.
  • the combined first and second polymers are extruded through a spinneret at a temperature of about 250 °C to about 275 °C, for example at least about 255 °C and up to about 270 °C.
  • the spun filaments are extruded in bundles comprising at least about 34 filaments per threadline, for example from about 175 filaments to about 6800 filaments, or even 6900 filaments or higher.
  • the undrawn filaments typically have a denier per filament in the range of about 3 to about 8, or more.
  • Spinneret orifices are typically round for round fiber cross-sections, but variously shaped orifices can be used as needed, for example for trilobal or delta cross-sections.
  • the spun filaments have a denier in the range of from about 3 to about 8 dpf and are collected as bundles (tow).
  • the tow has a dry heat shrinkage of less than 6% as determined by the Dry Heat Shrinkage Method disclosed herein in the Examples.
  • tow is fed from a set of cans or a creel containing undrawn melt spun yarns. Finish may be applied to facilitate processing downstream. Tow is then then drawn while immersed in a heated dilute finish water bath. In general feed roll is kept at room temperature while the draw roll may be heated. Drawn tow is stabilized by passing it through a saturated steam chamber and can be optionally further drawn and annealed over a number of heated draw roll modules before passing it over a room temperature roll module. Various simplifications of the draw zone are possible with less or more heater or room temperature draw module to optimally draw and stabilize yarn in preparation for crimping.
  • Crimping module typically uses a steam box that reduces yarn modulus in preparation for crimping, Typically, the crimper is a mechanical stuffer box type crimper with a flapper gate, acted upon by pneumatic pressure. Yarn tow is pulled into the crimper box by a set of driven rolls; yarn buckles and forms crimp as the flow out of the box is controlled by back pressure on the flapper. Crimped tow passes through an annealer section prior to being cut into staple.
  • the final denier per filament of the melt spun staple fiber may range from 1 -2 for cotton system processing and from 2-3 for wool system processing.
  • the melt spun staple fibers disclosed herein offer processing advantages.
  • the staple fiber can be processed with good productivity through opening, carding, and drawing steps in making spun yarns.
  • the melt spun staple fibers disclosed herein may be run on a staple spinning process using conditions typical for PET staple spinning.
  • the drawn fiber can be cut into staple of any desired length. If the staple fiber is too short, it can be difficult to card. If it is too long, it can be difficult to spin on cotton or woolen system equipment.
  • the staple fiber typically has a length in the range of from about 32 mm to about 51 mm, for example in the range of from about 38 to 40 mm.
  • the staple fiber typically has multiple cut lengths with an average cut length in the range of from about 70 mm to about 100 mm, for example in the range of from about 80 mm to about 90 mm.
  • the staple fiber can be crimped to have full sinus arc from about 10 to about 18, for example about 11 to about 15, crimps per inch.
  • melt spun staple fiber typically has 1 -2 denier per filament, a tenacity greater than 4 g/denier, and a break elongation of 20-60%, as determined using methods disclosed in the Examples herein below.
  • melt spun staple fiber typically has 2-4 denier per filament, a tenacity greater than 4 g/denier, and a break elongation of 30-90%.
  • the melt spun staple fiber disclosed herein can be used to make spun yarn.
  • the spun yarn consists essentially of the melt spun staple fiber, and does not contain any other type of staple fiber.
  • the spun yarn comprises the melt spun staple fiber disclosed herein.
  • the spun yarn further comprises a second staple fiber in an amount from about 5 weight percent to about 95 weight percent, based on the total weight of the spun yarn.
  • the second staple fiber can comprise at least one natural fiber.
  • the second staple fiber comprises at least one natural fiber selected from cotton, linen, wool, angora, mohair, alpaca, or cashmere.
  • the second staple can comprise at least one synthetic fiber.
  • the second staple fiber comprises polylactic acid, acrylic, nylon, olefin, acetate, rayon, or polyester.
  • the second staple fiber can comprise at least one regenerated cellulose fiber.
  • the term“regenerated cellulose fiber” means a textile fiber made from regenerated cellulose, also referred to as rayon, and includes lyocell, viscose, Modal®, and Tencel® fibers.
  • “lyocell” means a form of rayon which consists of cellulose fiber made from dissolving bleached wood pulp using dry jet-wet spinning.
  • “viscose” means a regenerated
  • Modal® means fiber made from wood pulp from beech trees.
  • “Tencel®” means fiber made from eucalyptus trees.
  • the spun yarn comprises melt spun staple fiber comprising a first polymer comprising PTT or PBT and a second polymer comprising PET or Co-PET, wherein the weight ratio of the first polymer to the second polymer is in the range of from about 80:20 to about 10:90, or about 70:30 to about 30:70, or about 60:40 to about 40:60; or about 70:30 to about 50:50, and the spun yarn further comprises a second staple fiber comprising cotton.
  • the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90, for example from about 90:10 to about 80:20, and the spun yarn further comprises a second staple fiber comprising cotton.
  • the cotton can be present in the spun yarn in an amount from about 5 wt% to about 95 wt%, and the melt spun staple fiber can be present in the spun yarn in an amount from about 95 wt% to about 5 wt%, based on the total weight of the spun yarn.
  • the spun yarn can contain about 5 wt% cotton and about 95 wt% melt spun staple fiber, or about 10 wt% cotton and about 90 wt% melt spun staple fiber, or about 15 wt% cotton and about 85 wt% melt spun staple fiber, or about 20 wt% cotton and about 80 wt% melt spun staple fiber, or about 25 wt% cotton and about 75 wt% melt spun staple fiber, or about 30 wt% cotton and about 70 wt% melt spun staple fiber, or about 35 wt% cotton and about 65 wt% melt spun staple fiber, or about 40 wt% cotton and about 60 wt% melt spun staple fiber, or about 45 wt% cotton and about 55 wt% melt spun staple fiber, or about 50 wt% cotton and about 50 wt% melt spun staple fiber, or about 55 wt% cotton and about 45 wt% melt spun staple fiber, or about 60 wt% cotton and about 40 wt% melt spun staple fiber, or about 65 wt% cotton, or
  • the spun yarn can comprise the melt spun staple fiber at greater than 95 wt% and the second staple fiber comprising cotton at less than 5 wt%.
  • the relative amounts of cotton and melt spun staple fiber are selected to provide desired characteristics to the spun yarn and fabrics made from the yarn.
  • the spun yarn can have a cotton count (Ne) of about 4 to about 70, for example from about 4 to about 60, or from about 4 to about 50, or from about 10 to about 60, or from about 20 to about 60.
  • the spun yarn comprising cotton can have a tenacity at break of at least 10 cN/tex. In some embodiments the spun yarn comprising cotton can have a tenacity at break of at least 10 cN/tex.
  • the spun yarn comprising cotton can have an elongation at break of at least 4%. Methods to determine tenacity and elongation at break are provided in the Examples herein below.
  • the spun yarn comprises melt spun staple fiber comprising a first polymer comprising PTT or PBT and a second polymer comprising PET or Co-PET, wherein the weight ratio of the first polymer to the second polymer is in the range of from about 80:20 to about 10:90, or about 70:30 to about 30:70, or about 60:40 to about 40:60; or about 70:30 to about 50:50, and the spun yarn further comprises a second staple fiber comprising wool.
  • the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90, for example from about 90:10 to about 80:20
  • the spun yarn further comprises a second staple fiber comprising wool.
  • the term“wool” refers to the fiber from fleece of sheep or lamb.
  • the wool can be present in an amount from about 5 wt% to about 95 wt%
  • the melt spun staple fiber can be present in an amount from about 95 wt% to about 5 wt%, based on the total weight of the spun yarn.
  • the spun yarn can contain about 5 wt% wool and about 95 wt% melt spun staple fiber, or about 10 wt% wool and about 90 wt% melt spun staple fiber, or about 15 wt% wool and about 85 wt% melt spun staple fiber, or about 20 wt% wool and about 80 wt% melt spun staple fiber, or about 25 wt% wool and about 75 wt% melt spun staple fiber, or about 30 wt% wool and about 70 wt% melt spun staple fiber, or about 35 wt% wool and about 65 wt% melt spun staple fiber, or about 40 wt% wool and about 60 wt% melt spun staple fiber, or about 45 wt% wool and about 55 wt% melt spun staple fiber, or about 50 wt% wool and about 50 wt% melt spun staple fiber, or about 55 wt% wool and about 45 wt% melt spun staple fiber, or about 60 wt% wool and about 40 wt% melt spun staple fiber, or about 65 wt% wool, or
  • the relative amounts of wool and melt spun staple fiber are selected to provide desired characteristics to the spun yarn and fabrics made from the yarn.
  • the spun yarn can have a worsted count (Nm) of about 7 to about 120, for example from about 7 to about 110, or from about 7 to about 100, or from about 10 to about 120, or from about 10 to about 100, or from about 10 to about 75.
  • the spun yarn comprises melt spun staple fiber comprising a first polymer comprising PTT or PBT and a second polymer comprising PET or Co-PET, wherein the weight ratio of the first polymer to the second polymer is in the range of from about 80:20 to about 10:90, or about 70:30 to about 30:70, or about 60:40 to about 40:60; or about 70:30 to about 50:50, and the spun yarn further comprises a second staple fiber comprising rayon.
  • the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90, for example from about 90:10 to about 80:20, and the spun yarn further comprises a second staple fiber comprising rayon.
  • “rayon” means textile fiber made from regenerated cellulose and includes lyocell, viscose, Modal®, and Tencel® fibers.
  • the rayon in the spun yarn, can be present in an amount from about 5 wt% to about 95 wt%, and the melt spun staple fiber can be present in an amount from about 95 wt% to about 5 wt%, based on the total weight of the spun yarn.
  • the spun yarn can contain about 5 wt% rayon and about 95 wt% melt spun staple fiber, or about 10 wt% rayon and about 90 wt% melt spun staple fiber, or about 15 wt% rayon and about 85 wt% melt spun staple fiber, or about 20 wt% rayon and about 80 wt% melt spun staple fiber, or about 25 wt% rayon and about 75 wt% melt spun staple fiber, or about 30 wt% rayon and about 70 wt% melt spun staple fiber, or about 35 wt% rayon and about 65 wt% melt spun staple fiber, or about 40 wt% rayon and about 60 wt% melt spun staple fiber, or about 45 wt% rayon and about 55 wt% melt spun staple fiber, or about 50 wt% rayon and about 50 wt% melt spun staple fiber, or about 55 wt% rayon and about 45 wt% melt spun staple fiber, or about 60 wt% rayon and about 40 wt% melt spun staple fiber, or about 65 wt% rayon, or
  • the relative amounts of rayon and melt spun staple fiber are selected to provide desired characteristics to the spun yarn and fabrics made from the yarn.
  • the spun yarn can have a cotton count (Ne) of about 4 to about 80, for example from about 10 to about 60, or from about 12 to about 40.
  • the spun yarn comprises melt spun staple fiber comprising a first polymer comprising PTT or PBT and a second polymer comprising PET or Co-PET, wherein the weight ratio of the first polymer to the second polymer is in the range of from about 80:20 to about 10:90, or about 70:30 to about 30:70, or about 60:40 to about 40:60; or about 70:30 to about 50:50, and the spun yarn further comprises a second staple fiber comprising acrylic.
  • the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90, for example from about 90:10 to about 80:20, and the spun yarn further comprises a second staple fiber comprising acrylic.
  • “acrylic fiber” means synthetic fibers made from a polyacrylonitrile having an average molecular weight of ⁇ 100,000, about 1900 monomer units.
  • the acrylic fiber can be present in an amount from about 5 wt% to about 95 wt%
  • the melt spun staple fiber can be present in an amount from about 95 wt% to about 5 wt%, based on the total weight of the spun yarn.
  • the spun yarn can contain about 5 wt% acrylic fiber and about 95 wt% melt spun staple fiber, or about 10 wt% acrylic fiber and about 90 wt% melt spun staple fiber, or about 15 wt% acrylic fiber and about 85 wt% melt spun staple fiber, or about 20 wt% acrylic fiber and about 80 wt% melt spun staple fiber, or about 25 wt% acrylic fiber and about 75 wt% melt spun staple fiber, or about 30 wt% acrylic fiber and about 70 wt% melt spun staple fiber, or about 35 wt% acrylic fiber and about 65 wt% melt spun staple fiber, or about 40 wt% acrylic fiber and about 60 wt% melt spun staple fiber, or about 45 wt% acrylic fiber and about 55 wt% melt spun
  • the relative amounts of acrylic fiber and melt spun staple fiber are selected to provide desired characteristics to the spun yarn and fabrics made from the yarn.
  • the spun yarn can have a cotton count (Ne) of about 4 to about 80, for example from about 10 to about 60, or from about 12 to about 40.
  • the spun yarn comprises melt spun staple fiber comprising a first polymer comprising PTT or PBT and a second polymer comprising PET or Co-PET, wherein the weight ratio of the first polymer to the second polymer is in the range of from about 80:20 to about 10:90, or about 70:30 to about 30:70, or about 60:40 to about 40:60; or about 70:30 to about 50:50, and the spun yarn further comprises a second staple fiber comprising polylactic acid (PLA).
  • the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene
  • the spun yarn further comprises a second staple fiber comprising PLA.
  • “polylactic fiber” means a manufactured fiber in which the fiber-forming substance is composed of at least 85% by weight of lactic acid ester units derived from naturally occurring sugars.
  • the PLA can be present in an amount from about 5 wt% to about 95 wt%, and the melt spun staple fiber can be present in an amount from about 95 wt% to about 5 wt%, based on the total weight of the spun yarn.
  • the spun yarn can contain about 5 wt% PLA and about 95 wt% melt spun staple fiber, or about 10 wt% PLA and about 90 wt% melt spun staple fiber, or about 15 wt% PLA and about 85 wt% melt spun staple fiber, or about 20 wt% PLA and about 80 wt% melt spun staple fiber, or about 25 wt% PLA and about 75 wt% melt spun staple fiber, or about 30 wt% PLA and about 70 wt% melt spun staple fiber, or about 35 wt% PLA and about 65 wt% melt spun staple fiber, or about 40 wt% PLA and about 60 wt% melt spun staple fiber, or about 45 wt%
  • PLA and about 55 wt% melt spun staple fiber or about 50 wt% PLA and about 50 wt% melt spun staple fiber, or about 55 wt% PLA and about 45 wt% melt spun staple fiber, or about 60 wt% PLA and about 40 wt% melt spun staple fiber, or about 65 wt% PLA and about 35 wt% melt spun staple fiber, or about 70 wt%
  • PLA and about 30 wt% melt spun staple fiber or about 75 wt% PLA and about 25 wt% melt spun staple fiber, or about 80 wt% PLA and about 20 wt% melt spun staple fiber, or about 85 wt% PLA and about 15 wt% melt spun staple fiber, or about 90 wt% PLA and about 10 wt% melt staple fiber, or about 95 wt% PLA and about 5 wt% melt spun staple fiber, based on the total weight of the spun yarn.
  • the relative amounts of PLA and melt spun staple fiber are selected to provide desired characteristics to the spun yarn and fabrics made from the yarn.
  • the spun yarn comprises melt spun staple fiber comprising a first polymer comprising PTT or PBT and a second polymer comprising PET or Co-PET, wherein the weight ratio of the first polymer to the second polymer is in the range of from about 80:20 to about 10:90, or about 70:30 to about 30:70, or about 60:40 to about 40:60; or about 70:30 to about 50:50, and the spun yarn further comprises a second staple fiber comprising nylon.
  • the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90, for example from about 90:10 to about 80:20, and the spun yarn further comprises a second staple fiber comprising nylon.
  • “nylon fiber” means a
  • the fiber-forming substance is a long chain synthetic polyamide in which less than 85% of the amide linkages are attached directly to two aliphatic groups.
  • the nylon can be present in an amount from about 5 wt% to about 95 wt%, and the melt spun staple fiber can be present in an amount from about 95 wt% to about 5 wt%, based on the total weight of the spun yarn.
  • the spun yarn can contain about 5 wt% nylon and about 95 wt% melt spun staple fiber, or about 10 wt% nylon and about 90 wt% melt spun staple fiber, or about 15 wt% nylon and about 85 wt% melt spun staple fiber, or about 20 wt% nylon and about 80 wt% melt spun staple fiber, or about 25 wt% nylon and about 75 wt% melt spun staple fiber, or about 30 wt% nylon and about 70 wt% melt spun staple fiber, or about 35 wt% nylon and about 65 wt% melt spun staple fiber, or about 40 wt% nylon and about 60 wt% melt spun staple fiber, or about 45 wt% nylon and about 55 wt% melt spun staple fiber, or about 50 wt% nylon and about 50 wt% melt spun staple fiber, or about 55 wt% nylon and about 45 wt% melt spun staple fiber, or about 60 wt% nylon and about 40 wt% melt spun staple fiber, or about 65 wt% nylon, or
  • the spun yarn comprises melt spun staple fiber comprising a first polymer comprising PTT or PBT and a second polymer comprising PET or Co-PET, wherein the weight ratio of the first polymer to the second polymer is in the range of from about 80:20 to about 10:90, or about 70:30 to about 30:70, or about 60:40 to about 40:60; or about 70:30 to about 50:50, and the spun yarn further comprises a second staple fiber comprising olefin.
  • the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90, for example from about 90:10 to about 80:20, and the spun yarn further comprises a second staple fiber comprising olefin.
  • “olefin fiber” means a
  • the fiber-forming substance is any long chain synthetic polymer composed of at least 85% by weight of ethylene, propylene, or other olefin units, except amorphous (noncrystalline) polyolefins qualifying as a rubber fiber.
  • the olefin fiber can be present in an amount from about 5 wt% to about 95 wt%, and the melt spun staple fiber can be present in an amount from about 95 wt% to about 5 wt%, based on the total weight of the spun yarn.
  • the spun yarn can contain about 5 wt% olefin fiber and about 95 wt% melt spun staple fiber, or about 10 wt% olefin fiber and about 90 wt% melt spun staple fiber, or about 15 wt% olefin fiber and about 85 wt% melt spun staple fiber, or about 20 wt% olefin fiber and about 80 wt% melt spun staple fiber, or about 25 wt% olefin fiber and about 75 wt% melt spun staple fiber, or about 30 wt% olefin fiber and about 70 wt% melt spun staple fiber, or about 35 wt% olefin fiber and about 65 wt% melt spun staple fiber, or about 40 wt% olefin fiber and about 60 wt% melt spun staple fiber, or about 45 wt% olefin fiber and about 55 wt% melt spun staple fiber, or about 50 wt% olefin fiber and about 50 wt% melt spun staple fiber
  • the spun yarn comprises melt spun staple fiber comprising a first polymer comprising PTT or PBT and a second polymer comprising PET or Co-PET, wherein the weight ratio of the first polymer to the second polymer is in the range of from about 80:20 to about 10:90, or about 70:30 to about 30:70, or about 60:40 to about 40:60; or about 70:30 to about 50:50, and the spun yarn further comprises a second staple fiber comprising acetate.
  • the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90, for example from about 90:10 to about 80:20, and the spun yarn further comprises a second staple fiber comprising acetate.
  • “acetate fiber” means a manufactured fiber in which the fiber-forming substance is cellulose acetate, and includes diacetate and triacetate. Diacetate is defined as cellulose acetate fiber for which more than 74% and less than 92% of the hydroxyl groups has been acetylated (degree of esterification above 2.22 and below 2.76).
  • Triacetate is defined as cellulose acetate fiber for which more than 92% of the hydroxyl groups has been acetylated (degree of esterification above 2.76 and below 3.00).
  • the acetate fiber can be present in an amount from about 5 wt% to about 95 wt%, and the melt spun staple fiber can be present in an amount from about 95 wt% to about 5 wt%, based on the total weight of the spun yarn.
  • the spun yarn can contain about 5 wt% acetate fiber and about 95 wt% melt spun staple fiber, or about 10 wt% acetate fiber and about 90 wt% melt spun staple fiber, or about 15 wt% acetate fiber and about 85 wt% melt spun staple fiber, or about 20 wt% acetate fiber and about 80 wt% melt spun staple fiber, or about 25 wt% acetate fiber and about 75 wt% melt spun staple fiber, or about 30 wt% acetate fiber and about 70 wt% melt spun staple fiber, or about 35 wt% acetate fiber and about 65 wt% melt spun staple fiber, or about 40 wt% acetate fiber and about 60 wt% melt spun staple fiber, or about 45 wt% acetate fiber and about 55 wt% melt spun staple fiber, or about 50 wt% acetate fiber and about 50 wt% melt spun staple fiber, or about 55 wt% acetate fiber and about 45 wt% melt spun
  • the spun yarn comprises melt spun staple fiber comprising a first polymer comprising PTT or PBT and a second polymer comprising PET or Co-PET, wherein the weight ratio of the first polymer to the second polymer is in the range of from about 80:20 to about 10:90, or about 70:30 to about 30:70, or about 60:40 to about 40:60; or about 70:30 to about 50:50, and the spun yarn further comprises a second staple fiber comprising a polyester, for example polyethylene terephthalate), poly(trimethylene
  • the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90, for example from about 90:10 to about 80:20
  • the spun yarn further comprises a second staple fiber comprising a polyester.
  • the polyester can be present in an amount from about 5 wt% to about 95 wt%
  • the melt spun staple fiber can be present in an amount from about 95 wt% to about 5 wt%, based on the total weight of the spun yarn.
  • the spun yarn can contain about 5 wt% polyester fiber and about 95 wt% melt spun staple fiber, or about 10 wt% polyester fiber and about 90 wt% melt spun staple fiber, or about 15 wt% polyester fiber and about 85 wt% melt spun staple fiber, or about 20 wt% polyester fiber and about 80 wt% melt spun staple fiber, or about 25 wt% polyester fiber and about 75 wt% melt spun staple fiber, or about 30 wt% polyester fiber and about 70 wt% melt spun staple fiber, or about 35 wt% polyester fiber and about 65 wt% melt spun staple fiber, or about 40 wt% polyester fiber and about 60 wt% melt spun staple fiber, or about 45 wt% polyester fiber and about 55 wt% melt spun staple fiber, or about 50 wt% polyester fiber and about 50 wt% melt spun staple fiber, or about 55 wt% polyester fiber and about 45 wt% melt spun staple fiber, or about 60 wt% polyester fiber and about 40 wt% melt melt spun
  • the relative amounts of polyester fiber and melt spun staple fiber are selected to provide desired characteristics to the spun yarn and fabrics made from the yarn.
  • the spun yarn can have a cotton count (Ne) of about 4 to about 80, for example from about 10 to about 60, or from about 12 to about 40.
  • the melt spun staple fibers are cut to lengths as desired for blending with a second fiber and subsequent processing on the cotton or woolen system.
  • spun yarns comprising the melt spun staple fiber and cotton, linen, polylactic acid, acrylic, nylon, olefin, acetate, polyester, or rayon fiber typically can be processed on the cotton system.
  • Spun yarns comprising the melt spun staple fiber and wool, angora, mohair, or cashmere fiber typically can be processed on the woolen system.
  • the melt spun staple fibers, and optionally at least one second staple fiber are first blended, for example by stack mixing, a process in which fiber bales are opened, mixed, and laid in layers.
  • Fiber bundles can be opened to smaller sized fiber tufts, for example in a blow room using a sequence of coarse opening machines followed by fine opening machines.
  • the smaller fiber bundles are then carded to form a continuous fiber strand, referred to as sliver, where almost all the fibers are oriented along the sliver axis.
  • Sliver from a carding machine can have very high mass/length variation, so typically a number of carding slivers (i.e.
  • the sliver delivered from the final draw frame has minimal mass/length variation but high linear density compared to the linear density desired in the final spun yarn, so the linear density of the sliver is reduced in a drawing process.
  • the drawing process is operated in two steps, in which partial drafting and twisting are performed to prepare the roving.
  • the roving is converted to spun yarn by drafting it further on a final spinning machine using known processes such as ring, open end, air jet, and vortex spinning.
  • the spun yarn can be wound onto a small package referred to as a cop in ring spinning; several cops can be joined and wound onto a larger final package referred to as a cone.
  • Woven and knitted fabrics can be made from the spun yarns disclosed herein.
  • Stretch fabric examples include circular, flat, and warp knits, and plain, twill, and satin wovens.
  • Articles such as garments can be made from fabrics comprising the spun yarns disclosed herein.
  • Nonwoven fabrics can be made from the staple fibers disclosed herein, and can be useful in articles such as wipes, diapers, napkins, and personal care items. Nonwoven fabrics can also be used as the base material for coated fabrics and in a variety of other applications, such as apparel and home furnishings.
  • spun yarns disclosed herein are useful in making fabrics, such as woven or knit fabrics.
  • a fabric comprising a spun yarn as disclosed herein is a woven fabric having a warp and a weft.
  • the warp comprises a spun yarn as disclosed herein.
  • the weft comprises a spun yarn as disclosed herein.
  • the warp and the weft each comprise a spun yarn as disclosed herein.
  • the woven fabric can further comprise additional yarns or continuous filament, for example in the warp, in the weft, or in both the warp and the weft.
  • spun yarn as disclosed herein is used in the warp, and a spun yarn comprising a natural fiber is used in the weft.
  • spun yarn as disclosed herein is used in the warp, and a spun yarn comprising a synthetic fiber is used in the weft.
  • a spun yarn comprising a natural fiber is used in the warp and a spun yarn as disclosed herein is used in the weft.
  • a spun yarn comprising a synthetic fiber is used in the warp and a spun yarn as disclosed herein is used in the weft.
  • spun yarn as disclosed herein is used in the warp and also in the weft. Knit fabrics can be made using only the spun yarns disclosed herein, or in conjunction with a spun yarn comprising a natural or a synthetic fiber.
  • Woven fabrics comprising spun yarns as disclosed herein can have a fabric weight in the range of about 80 g/m 2 to about 600 g/m 2 , for example.
  • Fabrics comprising spun yarns as disclosed herein can offer advantages over fabrics of the same construction consisting of spun yarns of PET, cotton, rayon, PTT, or a combination thereof, and lacking the melt spun staple fibers disclosed herein.
  • fabrics comprising spun yarns comprising melt spun staple fibers as disclosed herein can have softer hand (i.e. feel softer) than fabrics of PET, cotton, rayon, or a combination thereof, as well as greater bulk, as indicated by greater fabric thickness.
  • Fabrics comprising the spun yarns disclosed herein can have better dyeability than a fabric of the same construction consisting of PET, cotton, rayon, or a combination thereof.
  • the fabrics disclosed herein can dye more deeply, darker, and at lower temperatures.
  • the fabrics disclosed herein can have better dye pickup than PET fabrics when dyed at a lower temperature, which offers reduced cost through energy savings.
  • fabrics containing the spun yarns disclosed herein can dye darker (i.e. have lower L* values when measured under a D65 light source) than PET fabrics when dyed simultaneously, and can dye darker than PET fabric even when dyed at 100 °C and with comparison PET fabrics dyed at 130 °C.
  • the properties of picking up more dye, picking up dye at lower temperature, and dyeing more deeply can be referred to as“better dyeability” of a fabric.
  • the woven fabrics disclosed herein can also have improved drape, for example as demonstrated by higher area of drape and drape coefficient values, for example as determined by method BS 5058. Especially desirable in a fabric is the combination of softer hand and improved drape.
  • the fabrics disclosed herein demonstrated less pilling (higher pill rating values) than fabrics of the same construction consisting of PET, cotton, rayon, or a combination thereof, for example as determined by the ASTM D4970 method, and better abrasion resistance.
  • the fabrics disclosed herein can also have better tear strength in the warp and/or weft direction than fabrics of the same construction consisting of PET, cotton, rayon, or a combination thereof.
  • Knit fabrics comprising spun yarns as disclosed herein can have higher recovery than a knit fabric of the same construction consisting of polyethylene
  • a spun yarn comprising: melt spun staple fiber comprising a first polymer comprising poly(trimethylene terephthalate) (PTT) or poly(butylene terephthalate) (PBT) and a second polymer comprising polyethylene terephthalate) (PET) or Co-PET, wherein Co-PET is a poly(ethylene terephthalate) copolymer comprising isophthalic acid monomer; and wherein the first polymer comprises
  • poly(trimethylene terephthalate) and the weight ratio of the poly(trimethylene terephthalate) to the second polymer is in the range of from about 80:20 to about 10:90; or the first polymer comprises poly(butylene terephthalate) and the weight ratio of the poly(butylene terephthalate) to the second polymer is in the range of from about 90:10 to about 10:90.
  • the spun yarn of embodiment 1 or 4 wherein the first polymer comprises poly(butylene terephthalate) and the second polymer comprises Co-PET. 6.
  • the spun yarn of embodiment 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, or 11 further comprising a second staple fiber in an amount from about 5 wt% to about 95 wt%, based on the total weight of the spun yarn.
  • the spun yarn of embodiment 12, wherein the second staple fiber comprises polylactic acid, acrylic, nylon, olefin, acetate, rayon, polyester, cotton, linen, wool, angora, mohair, alpaca, cashmere, or a mixture thereof.
  • the spun yarn of embodiment 12, 13, or 14, wherein the second staple fiber comprises wool. 18.
  • a fabric comprising a spun yarn of embodiment 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13, 14, 15, 16, 17, or 18.
  • Standard Test Method than a fabric of the same fabric construction consisting of polyethylene terephthalate, cotton, rayon, or a combination thereof.
  • a fabric of embodiment 26, wherein the warp comprises a spun yarn of embodiment 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13, 14, 15, 16, 17, or 18.
  • a fabric of embodiment 26 or 27, wherein the weft comprises a spun yarn of embodiment 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13, 14, 15, 16, 17, or 18.
  • melt spun staple fiber comprising a first polymer comprising
  • a weight ratio of poly(butylene terephthalate) to the second polymer in the range of from about 90: 10 to about 10:90;
  • melt spun staple fiber of embodiment 34 wherein the weight ratio of the poly(trimethylene terephthalate) or the poly(butylene terephthalate) to the second polymer is in the range of about 70:30 to about 50:50.
  • “Comp. Ex.” Means Comparative Example;“Ex.” means Example;“rpm” means revolutions per minute;“wt%” means weight percent; “dL/g” is deciliters per gram;“g” is gram(s);“mg” is millligram(s);“°C” means degrees Celsius;“min” is minute(s);“h” is hour(s);“s” is second(s);“lb” is pound(s); “kg” is kilogram(s);“mm” is millimeter(s);“m” is meter(s);“gpl” is grams per liter;“m/min” is meters per minute;“mol” is mole;“kg” is kilogram(s); “ppm” is parts per million; “Hz” is hertz;“cN” is centiNewton(s); “rpm” is revolutions per minute; “wt” is weight;“dpf” is denier per filament; “g/d” is grams per denier;“Ne” means
  • Polytrimethylene terephthalate (PTT) containing 0.3% T1O2 and having an intrinsic viscosity of 0.96 dL/g was obtained from E.l. du Pont de Nemours and Company (Wilmington, DE) as merge K2266.
  • Co-PET containing 1.7 mol% of isophthalic acid (IPA) monomer, 48.4 mol% of terephthalic acid (TPA) monomer, and 49.9 mol% of ethylene glycol (EG) monomer was obtained from Nan Ya Plastics Corporation, America, P.O. Box 939, Lake City, S.C 29560, USA.
  • the Co-PET composition was determined by NMR analysis and is given based on the total copolymer composition.
  • the Co-PET had an intrinsic viscosity of 0.80 dL/g.
  • Fiber-grade post-consumer recycled Co-PET containing 1.1 mol % IPA monomer, 49.1 mol % TPA monomer, and 49.9 mol% of EG monomer was obtained from William Barnet & Son, LLC, P.O. Box 171898, Spartanburg, S.C. 29301 , USA.
  • the Co-PET composition was determined by NMR analysis and is given based on the total copolymer composition.
  • the Co-PET had an intrinsic viscosity of 0.76 dL/g.
  • Co-PET composition was determined by NMR analysis using the following procedure. The Co-PET pellets were cryoground into a powder-like form, then ⁇ 18 mg were weighed into an NMR tube and a solution of 5:1
  • CDCh:TFA-D (5:1 deuterated chloroform/deuterated trifluoroacetic acid) added to 0.6 mL total volume. The sample was vortexed to dissolve the Co-PET. A proton NMR spectrum was obtained within 30 minutes of dissolution.
  • Proton NMR spectra were acquired on a 500 MHz Bruker Avance III HD NMR equipped with 5 mm CPQCI (indirect) cryoprobe at 30 °C. The following parameters were used for acquisition: recycle delay of 30 seconds, acquisition time of 4 sec, 90 degree pulse of 8.0 seconds, spectral window of 10000 Hz, 79998 points, a total of 64 scans/transients collected and averaged. The spectrum is referenced to chloroform-d residual proton signal at 7.24 ppm, and processed with lb of 0.10 Hz and zero-filled out to 512k.
  • Co-PET composition was calculated from integrals for the signals at approximately 8.7 ppm, 8.1 ppm, and 4.8 ppm corresponding to isophthalic acid, terephthalic acid, and ethylene glycol between terephthalic acid groups, respectively.
  • the isophthalic acid signal used represents 1 mole of protons, so its integral was already relative.
  • the terephthalic acid integral represents 4 moles of terephthalic acid protons and includes 2 moles of isophthalic acid protons; the terephthalic acid relative integral was determined by subtracting 2x the isophthalic acid relative integral, then dividing the remainder by 4.
  • the ethylene glycol-related integral corresponds to 4 moles of ethylene glycol protons, and the relative integral was determined by dividing the measured integral by 4.
  • the three relative integrals were totaled, and the relative mol% values were calculated as each corresponding relative integral divided by the total, then multiplied by 100%.
  • Dry Heat Shrinkage of undrawn melt spun fiber was determined using the following procedure, which is referred to herein as Dry Heat Shrinkage Method.
  • Crimp contraction is the difference in length of a crimped versus de-crimped fiber. Measuring crimped length, L0, under a low load of 0.001 cN/dtex and de-crimped length, L1 , under a heavy load of 0.1 cN/dtex allows one to calculate crimp contraction as [(L1 - L0)/L1 ]*100.
  • Crimp stability is a measure of stability of crimp under a specified load. It can be measured by determining recovery in staple length when a load is removed. With L2 as the length of staple fiber (measured under 0.001 cN/dtex) 60 sec after a heavier load of 0.1 cN/dtex is applied for 10 sec (to determine L1 ), crimp stability can be calculated as [(L1 -L2/(L1 -L0)]*100.
  • Crimp recovery is the difference in length of a de-crimped fiber, L1 , and the fiber length after releasing the crimp removal force, L2, expressed as a percentage of de-crimped fiber: [(L1 -L2)/L1 ]*100.
  • Polytrimethylene terephthalate (PTT) containing 0.3% T1O2 and having an intrinsic viscosity of 0.96 dL/g was dried at 120 °C under nitrogen blanket in a vacuum oven for 16 hours and melt-extruded into round cross-section, 34- filament yarn bundle using a twin-screw extruder spinning machine. Extruder melt zone temperatures were maintained from 180-255 °C. Polymer throughput was 14.06 g/min with a winder speed of 1250 m/m giving a spun denier per filament of 2.9.
  • Dry heat shrinkage of yarn bundle was determined to be 47%.
  • Polytrimethylene terephthalate containing 0.3% T1O2 and having an intrinsic viscosity of 0.96 dL/g was melt blended with polyethylene terephthalate co-ethylene isophthalate (Co-PET) (from Nan Ya Plastics) having an intrinsic viscosity of 0.80 dL/g in a twin-screw extruder in a 50/50 weight ratio to form compounded pellets.
  • Extruder throughput was 150 Ib/h (68.04 kg/h, 0.0189 kg/s) and melt temperature at extruder exit was under 285 °C as measured by a hand- held thermocouple.
  • Polytrimethylene terephthalate containing 0.3% T1O2 and having an intrinsic viscosity of 0.96 dL/g was melt blended with fiber-grade post-consumer recycled Co-PET containing 1.1 mol % IPA monomer, 49.1 mol % TPA monomer, and 49.9 mol% of EG monomer in a twin-screw extruder in a 50/50 weight ratio to form compounded pellets.
  • the Co-PET had an intrinsic viscosity of 0.76 dL/g.
  • Extruder throughput was 150 Ib/h (0.0189 kg/s) and melt temperature at extruder exit was under 285 °C as measured by a hand-held thermocouple.
  • Polytrimethylene terephthalate containing 0.3% T1O2 and having an intrinsic viscosity of 0.96 dL/g was melt blended with Co-PET (from Nan Ya Plastics) in a twin-screw extruder in a 50/50 weight ratio to form compounded pellets.
  • Extruder throughput was 150 Ib/h (0.0189 kg/s) and melt temperature at extruder exit was under 285 °C as measured by a hand-held thermocouple.
  • Compounded material was at 145 °C for 20 hours.
  • Schill+Seilacher at 22 °C. Tow was first drawn, in a 0.5% concentration finish bath at 80 °C between a 22 °C feed roll running at 36 m/m and heated draw rolls at 75 °C running at 110.88 m/m giving a first stage draw ratio of 3.08. Drawn tow was pulled through a steam chest at 100 °C by a downstream heated roll at 165 °C and running at 110.88 m/m. Tow was passed over another set of rolls heated at 165 °C running at 99.8 m/m. Finish (6% concentration) was sprayed and tow was passed over cooling drum rolls at 25 °C, running at 99.8 m/m.
  • Crimper speed was 100 m/m.
  • Crimper roller temperature and pressure was 65 °C and 0.8 bar, respectively.
  • Crimped tow was annealed for 8 min at 100 °C in a plate belt drier, Crimped tow was finally cut to produce staple melt spun fiber having the following properties:
  • Polytrimethylene terephthalate containing 0.3% T1O2 and having an intrinsic viscosity of 0.96 dL/g was melt blended with Co-PET (from Nan Ya Plastics) in a twin-screw extruder in a 50/50 weight ratio to form compounded pellets.
  • Extruder throughput was 150 Ib/h (0.0189 kg/s) and melt temperature at extruder exit was under 285 °C as measured by a hand-held thermocouple.
  • Compounded material was at 145 °C for 20 hours.
  • Tow was first drawn in a 0.5% concentration finish bath at 80 °C between a 22 °C feed roll running at 30 m/m and heated draw rolls at 75 °C running at 109.3 m/m giving a first stage draw ratio of 3.64. Tow was pulled by a
  • Table 3 lists commercially obtained spun yarns and the abbreviations used for them in the Tables which follow. Some of these yarns were used to prepare the fabrics of the Comparative Examples.
  • Example 3 Melt spun staple fiber from Example 3 was used to prepare the spun yarns of Examples 5-10.
  • Tenacity was measured at 5 m/min using CRE type tensile testing equipment (such as Uster Tensorapid -3) at jaw speed of 5 m/min and specimen length of 50 cm.
  • CRE type tensile testing equipment such as Uster Tensorapid -3
  • CRE type tensile testing equipment such as Uster Tensorapid -3
  • Spun yarn was made using the cotton spinning system, according to the following procedure.
  • Melt spun staple fiber from Example 3 was taken from bales and hand mixed.
  • the average staple fiber length was 40 mm and the denier was 1.2 D.
  • the fibers were mixed and laid in layers in a stack mixing process, then conditioned at 65% relative humidity and 25 °C for 24 hours. Fiber mass was taken from the stack by vertically withdrawing material and feeding it to a blow room line as typically used to spin synthetic fibers. In this process, the size of a fiber tuft was broken down from about 150 mg to about 30 mg. The following parameters were used:
  • Feed Plate and Licker in gauge 32 thou (thousandths of an inch)
  • the roving was found to have Uster value (unevenness) of 3.16% and Uster % (unevenness %) of 3.26.
  • the roving was drafted further on a ring frame spinning machine to produce spun yarn having a yarn count of 20s Ne.
  • the following parameters were used:
  • roller gauge 42.5/65 mm
  • the spun yarn was wound at ring frame on small packages called cops, each weighing about 50 g. Many cops were joined and cleared for any yarn defect, and finally wound into a cone on a winding machine using the following parameters:
  • the final spun yarn was evaluated for tensile properties and unevenness % on Uster tensorapid-3 and Uster unevenness tester-3. Results are shown in Table 4.
  • the yarn wound in the final machine was lively and could snarl as a result of twist imparted in the spinning process.
  • the yarn was rendered structurally stable by conditioning the cone in an autoclave at a maximum temperature of 70 °C for 50 minutes.
  • Spun yarn was prepared using melt spun staple fiber from Example 3 according to the procedure of Example 5 except with the following differences:
  • the linear density of the final sliver was 4.75 g/meter and the Unevenness % was 1.75
  • Roving was prepared as in Example 5 except that the roving hank was 1.2 s Ne.
  • the twist multiplier/twist per inch was 3.6/22.6
  • the Traveler size was 4/0 M1 HO
  • the spindle speed was 16500 rpm.
  • the spun yarn was wound onto a cone at 1500 meters/min.
  • Spun yarn was prepared using melt spun staple fiber from Example 3 and cotton (Shankar 6 variety Indian cotton obtained from north Indian states, for example Punjab and Haryana).
  • the cotton staple had average length of 31 mm and fineness (fiber linear density) of 4.1 microgram/inch, measured using an airflow method.
  • the spun yarn was made according to the procedure of
  • Example 5 except with the following differences: In the hand mixing step, two layers of cotton sliver, taken from 100% cotton yarn spinning process after the combing machine and broken into small tuft size of 25-30 mg, were laid over one layer of melt spun staple fiber.
  • the linear density of the final sliver from the carding step was 4.7 g/meter.
  • Roving was prepared as in Example 5 except that the twist multiplier was 0.85 and the roving hank was 0.7 s Ne.
  • the roving was drafted further as in Example 5 except with twist per inch of 16.99.
  • Spun yarn was prepared using melt spun staple fiber from Example 3 and cotton (Shankar 6 variety Indian cotton commercially obtained from north Indian states).
  • the cotton staple had average length of 31 mm and linear density of 4.1 microgram/inch.
  • the spun yarn was made according to the procedure of
  • the linear density of the final sliver from the carding step was 4.7 g/meter.
  • Roving was prepared as in Example 5 except that the twist multiplier was 0.85 and the roving hank was 1.2 s Ne.
  • the roving was drafted further as in Example 5 except with twist per inch of 24.02, traveler size 4/0 M1 HO, and spindle speed 16500 rpm.
  • the spun yarn was wound onto a cone at 1500 meters/min.
  • Spun yarn was prepared using melt spun staple fiber from Example 3 and commercially-obtained Tencel® staple fiber (Lenzing).
  • the Tencel® staple fiber had average length of 40 mm and denier of 1.2 D.
  • the spun yarn was made according to the procedure of Example 5 except with the following differences:
  • the linear density of the final sliver from the carding step was 4.7 g/meter.
  • the roving was drafted further as in Example 5 except with twist per inch of 16.99.
  • Spun yarn was prepared using melt spun staple fiber from Example 3 and commercially-obtained Tencel® staple fiber (Lenzing).
  • the Tencel® staple had average length of 40 mm and denier of 1.2 D.
  • the spun yarn was made according to the procedure of Example 5 except with the following differences:
  • the linear density of the final sliver from the carding step was 4.7 g/meter.
  • Roving was prepared as in Example 5 except that twist multiplier was 0.85 and the roving hank was 1.2 s Ne.
  • the roving was drafted further as in Example 5 except with twist per inch of 24.02, traveler size 4/0 M1 HO, and spindle speed 16500 rpm.
  • the spun yarn was wound onto a cone at 1500 meters/m in. Properties of the spun yarn are given in Table 4. Table 4. Properties of the Spun Yarns of Example 5 Through Example 10 and of Comparative Spun Yarns Obtained Commercially
  • Spun yarns (Examples 5 and 6) consisting of only the melt spun staple fiber of Example 3, polyethylene terephthalate) staple, or poly(trimethylene terephthalate) staple were subjected to a boiling water shrinkage test method according to ASTM D2259.
  • PET spun yarns and PTT spun yarn were obtained commercially.
  • Pill rating 1000 rounds
  • Drape - BS 5058 Method for the Assessment of Drape of Fabrics
  • Bursting Strength (circular knits) - ASTM D3786 Standard Test Method for Bursting Strength of Textile Fabrics
  • Shrinkage % (in fabric, greige to finished) was determined as follows. Greige fabric was marked with a permanent marker to indicate a 30 cm line in the fabric length (warp direction) and a 30 cm line in the fabric width (weft direction). The fabric was then dyed and finished, and the lengths of the permanent marker lines were remeasured. For each of the length (warp) and width (weft) directions, percent shrinkage was calculated by dividing the difference in length of the line before and after dyeing and finishing by 30 and multiplying by 100. This method is referred to herein as the Percent Shrinkage Method.
  • Softness assessment also referred to as subjective Hand Value
  • the subjective hand value assessment was done by assessing the feel of the fabric by 12 experts in the field, tested in South India Textile Research Association (SITRA), Coimbatore, India. This is the method widely used in Textile Industry for assessment of softness of fabrics. Fabrics were coded A and B and given to assess the ranking of fabric based on the perception of Fabric softness independently. The Softer fabric was ranked where as less soft fabric was ranked‘2’ by each expert. This was done for 100 % PET fabrics and the fabrics of Examples 11 and 14. Final ranking was done by averaging the 12 readings. The fabric with lower rank average was given final rank as 1 (softer) and fabric with higher rank average was given as rank 2.
  • the spun yarns of Examples 5 through 10 were used to make woven fabrics as indicated in Table 6.
  • Woven twill (3/1 ) bottom weight fabrics and plain weave (1/1 ) shirting fabrics were made using the spun yarns disclosed herein as the warp and weft (fill) yarns; comparison fabrics were made using spun yarns obtained commercially in the warp and weft.
  • the same yarn was used in both the warp and the weft.
  • Fabric evaluation results are presented in Tables 7 and 8. Results are reported for finished fabric unless otherwise noted.
  • Spun yarn from Example 5 was used as the warp and as the weft to prepare a bottom weight woven twill fabric.
  • the warp yarns were sized before beaming using a CCI single end sizing machine using Elvanol-T25 PVA sizing agent. Using a warper at 350 m/min, a final beam with 2150 ends, a width of 18 inches, and end lengths of 3.5 meters was prepared. With the following denting plan:
  • 3/1 LHT twill fabric was woven on a CCI sample loom with loom speed at 40 picks/minute. The pick value was set at 63 picks / inch. Greige fabric of 2 m length and 49.5 cm width was obtained.
  • the greige fabric was desized on an RBE lab Jigger machine as follows.
  • the fabric sample was loaded into the jigger filled with water (2 L), NaOH (2 gpl), and wetting agent; Levocol CESR (wetting agent) was added (5 gpl) and the bath temperature was raised to 90 °C.
  • the fabric was run in the bath for 60 mins, then the bath was drained, refilled with fresh water, and the temperature of the bath was raised to 85 °C.
  • the fabric was hot water washed for 15 min, and the bath was drained.
  • the bath was again filled with water and the fabric was run through it for 15 min (cold water wash).
  • the fabric was then dyed with a mixture of disperse dyes using the following time and temperature profile: heat to 70 °C and hold for 10 minutes, then raise temperature 1.5 °C/min to 130 °C and hold for 30 minutes, then decrease temperature 1.5 °C/.min to 70 °C and drain.
  • Post dyeing the fabric was given a reduction cleaning with Hydros and NaOH (2 gpl each), 90 °C for 20 min.
  • the fabric was then washed with cold water for 10 minutes, contacted with acetic acid (2 gpl) for 15 minutes, then washed with cold water for 10 minutes.
  • the dyed fabric was padded with finishing agent (softener), then heat set at 160 °C for 45 seconds in an RBE lab stenter.
  • a comparative bottom weight woven 3/1 LHT twill fabric was made using commercially available 20s Ne 100% PET staple spun yarn (“P1”) as the warp and as the weft, following the procedure of Example 11 except that the denting plan used 4 ends / dent and the reed count was 50 dents / 2 inch.
  • the greige fabric was dyed, finished, and heat set as for Example 11.
  • Spun yarn from Example 7 was used as the warp and as the weft to prepare a bottom weight woven twill fabric according to the procedure of
  • Example 11 but with the following exceptions.
  • the greige fabric was desized and bleached in a Jigger machine, heat set in a stenter, then dyed with a mixture of disperse dyes, then additionally dyed with a reactive dye under cotton dyeing conditions.
  • a comparative bottom weight woven 3/1 LFIT twill fabric was made as in Example 12 except using commercially available 20s Ne 40/60 PET/cotton staple spun yarn (“PC1”) as the warp and as the weft.
  • PC1 Ne 40/60 PET/cotton staple spun yarn
  • Spun yarn from Example 9 was used as the warp and as the weft to prepare a bottom weight woven twill fabric according to the procedure of
  • Example 12 except that no peroxide killer was used at the end of the bleaching step.
  • a comparative bottom weight woven 3/1 LHT twill fabric was made following the procedure of Example 12 except using commercially available 20s Ne 40/60 PET/Tencel® staple spun yarn (“PT1”) as the warp and as the weft.
  • PT1 PET/Tencel® staple spun yarn
  • the greige fabric was dyed, finished, and heat set as for Example 12 except that the second dyeing step, with a reactive dye, was done under Tencel® dyeing conditions.
  • Spun yarn from Example 6 was used as the warp and as the weft to prepare a plain weave shirting fabric. The procedure was as described for Example 11 but with the following differences: after warping, the beam contained 1680 ends, and the reed count was 84 dents / 2 inch.
  • Example 14 In comparison to the fabric of Comparative Example E, the fabric of Example 14 was found to have a better (softer) hand. Other fabric properties are presented in Tables 7 and 8.
  • a comparative plain weave shirting fabric was made following the procedure of Example 11 except using commercially available 40s Ne 100% PET staple spun yarn (“P2”) as the warp and as the weft. After warping, the beam contained 1680 ends, and the reed count was 84 dents / 2 inch. Greige fabric of 2 m length and 47.7 cm was obtained.
  • Spun yarn from Example 8 was used as the warp and as the weft to prepare a plain weave shirting fabric.
  • the procedure was as described for Example 12, except that no peroxide killer was used at the end of the bleaching step. Fabric construction is shown in Table 6. Wicking test results were 100%. Other fabric properties are presented in Tables 7 and 8.
  • a comparative plain weave shirting fabric was made following the procedure of Example 11 except using commercially available 40s Ne 40/60 PET/cotton staple spun yarn (“PC2”) as the warp and as the weft and with the following additional differences in procedure: after warping, the beam contained 1748 ends, and the reed count was 92 dents / 2 inch. Greige fabric of 2 m length and 48.7 cm width was obtained, and was dyed as described in Example 12.
  • PC2 Ne 40/60 PET/cotton staple spun yarn
  • Spun yarn from Example 10 was used as the warp and as the weft to prepare a plain weave shirting fabric.
  • the procedure was as described for Example Wfab-1 , except that after warping the beam contained 1748 ends, the reed count was 92 dents / 2 inch, and the pick value was set at 62 picks / inch.
  • Greige fabric of 2 m length and 48.7 cm width was obtained, and was dyed as described in Example 12.
  • a comparative shirting fabric was made following the procedure of Example 11 except using commercially available 40s Ne 40/60 PET/Tencel® staple spun yarn (“PT2”) as the warp and as the weft and with the following additional differences in procedure: after warping, the beam contained 1748 ends, the reed count was 92 dents / 2 inch, and the pick value was set at 62 picks / inch. Greige fabric of 2 m length and 48.7 cm width was obtained and dyed as described in Example 12.
  • PT2 PET/Tencel® staple spun yarn
  • the spun yarns of Examples 5 through 10 were used as the knitting yarn to make circular knit fabrics as indicated in Table 9; comparison fabrics were made using spun yarns obtained commercially. For all circular knit fabrics made using 20s Ne count yarns, the machine gauge was 20”. For all circular knit fabrics made using 40s Ne count yarns, the machine gauge was 24”. Fabric evaluation results are presented in Tables 9 and 10. Results are reported for finished fabric unless otherwise noted.
  • Spun yarn from Example 5 was used to prepare a circular knit fabric on a Mesdan lab knitter.
  • the greige fabric was heat set in an RBE stenter at 160 °C for 45 seconds, then scoured in an HTHP Beaker dyeing machine using the following procedure.
  • the fabric was scoured at 90 °C for 60 minutes with NaOFI (2 gpl) and wetting agent Levocol CESR (5 gpl) added.
  • the fabric was washed at 85 °C for 15 minutes, then with cold water for 15 minutes, then with a neutralization solution containing acetic acid (1 gpl) for 15 minutes, followed by another cold water wash for 15 minutes.
  • the scoured fabric was then dyed in the same machine with a mixture of disperse dyes using the following time and temperature profile: heat to 70 °C and hold for 10 minutes, then raise temperature 1.5 °C/min to 130 °C and hold for 30 minutes, then decrease temperature 1.5 °C/.min to 70 °C and drain.
  • Post dyeing the fabric was given a reduction cleaning with Hydros and NaOH (2 gpl each), 90 °C for 20 min.
  • the fabric was then washed with cold water for 10 minutes, neutralized with acetic acid (2 gpl) for 15 minutes, then washed again with cold water for 10 minutes.
  • the dyed fabric was padded with finishing agent (softener), then heat set at 160 °C for 45 seconds in a lab stenter.
  • Example 17 In comparison to the fabric of Comparative Example H, the fabric of Example 17 was found to have a softer hand (i.e. better softness). Other fabric properties are presented in Tables 9 and 10.
  • a comparative knit fabric was made using following the procedure of Example 17 except that commercially available 20s Ne 100% PET staple spun yarn (“P1”) was used.
  • Spun yarn from Example 7 was used to prepare a circular knit fabric on a Mesdan lab knitter following the procedure of Example 17, except that after dyeing with the disperse dyes, the fabric was dyed in the same machine with a reactive dye mixture to which salt (60 gpl) was added, using the following time and temperature profile: heat to 60 °C and hold for 30 minutes, then add soda ash (15 gpl) and hold for 30 minutes before draining. The fabric was then washed with cold water for 10 minutes, washed with acetic acid (1 gpl) for 15 minutes, then given a hot soaping with Albatex AD (2 gpl) during which the temperature was raised to 90 °C and held for 15 minutes.
  • salt 60 gpl
  • the fabric was then washed with hot water (85 °C) for 15 minutes, and then with cold water for 10 minutes.
  • the dye was fixed with Levocol HCF (0.5 gpl) during which the temperature was raised to 50 °C and held for 20 minutes.
  • the dyed fabric was padded with finishing agent then heat set at 160 °C for 45 seconds in a lab stenter.
  • a comparative knit fabric was made using following the procedure of Example 18 except that commercially available 20s Ne 40/60 PET/cotton staple spun yarn (“PC1”) was used.
  • PC1 Ne 40/60 PET/cotton staple spun yarn
  • Spun yarn from Example 9 was used to prepare a circular knit fabric on a Mesdan lab knitter following the procedure of Example 18.
  • a comparative knit fabric was made using following the procedure of Example 18 except that commercially available 20s Ne 40/60 PET/Tencel® staple spun yarn (“PT1”) was used.
  • PT1 Ne 40/60 PET/Tencel® staple spun yarn
  • Spun yarn from Example 6 was used to prepare a circular knit fabric on a Mesdan lab knitter following the procedure of Example 1 except that a different mixture of disperse dyes was used.
  • Example 20 In comparison to the fabric of Comparative Example K, the fabric of Example 20 was found to have a better hand (i.e. better softness). Other fabric properties are presented in Tables 9 and 10.
  • Comparative Example K A comparative knit fabric was made using following the procedure of Example 17 except that commercially available 40s Ne 100% PET staple spun yarn (“P2”) and a different mixture of disperse dyes were used.
  • Spun yarn from Example 8 was used to prepare a circular knit fabric on a Mesdan lab knitter following the procedure of Example 18, except that a different mixture of disperse dyes was used.
  • a comparative knit fabric was made using following the procedure of Example 18 except that commercially available 40s Ne 40/60 PET/cotton staple spun yarn (“PC2”), a different mixture of disperse dyes, and a different mixture of reactive dyes used were used.
  • PC2 Ne 40/60 PET/cotton staple spun yarn
  • Spun yarn from Example 10 was used to prepare a circular knit fabric on a Mesdan lab knitter following the procedure of Example 18, except with a different mixture of disperse dyes and a different mixture of reactive dyes.
  • a comparative knit fabric was made using following the procedure of Example 18 except that commercially available 40s Ne 40/60 PET/Tencel® staple spun yarn (“PT2”), a different mixture of disperse dyes, and a different reactive dye were used.
  • PT2 Ne 40/60 PET/Tencel® staple spun yarn
  • the results in Tables 9 and 10 demonstrate that the circular knit fabrics of the Examples provide advantages over the fabrics of the Comparative Examples.
  • the circular knit fabrics containing spun yarns comprising the melt spun staple fibers disclosed herein have greater bulk in comparison to the fabrics of the Comparative Examples, as shown by the greater thickness of the fabrics.
  • the circular knit fabrics of the Examples also demonstrate less pilling (higher pill rating values) and better abrasion resistance (lower % weight loss). Additionally, the fabrics of the Examples have better stretch recovery than the Comparative Example fabrics, both at shorter and longer recovery times.
  • Spun yarn was made using the worsted spinning system, according to the following procedure.
  • melt spun staple fiber from Example 4 was used to prepare the spun yarn of Example 23.
  • the nominal count spun for the spun yarn was 2/64s Nm.
  • Spun yarn from Example 23 was used as the warp and as the weft to prepare a bottom weight twill fabric.
  • the warp yarns were sized before beaming using a CCI single end sizing machine using Elvanol-T25 PVA sizing agent and a softener. Using a warper at 350 m/min, a final beam with 1770 ends, a width of 18 inches, and end lengths of 3.5 meters was prepared. With the following denting plan:
  • the greige fabric was desized in a Jigger machine using a procedure similar to that of Example 11 , except that Albatex AD was used in conjunction with Levocol CESR.
  • the fabric was then subjected to a hot water wash (85 °C for 15 minutes), a cold water wash (15 minutes), a neutralization step with acetic acid (15 minutes), and another cold water wash (15 minutes).
  • the fabric was allowed to dry flat in atmospheric conditions, then heat set at 170 °C for 45 seconds.
  • the fabric was then dyed with a mixture of disperse dyes using the following time and temperature profile: heat to 70 °C and hold for 10 minutes, then raise temperature 1.5 °C/min to 130 °C and hold for 30 minutes, then decrease temperature 1.5 °C/.min to 70 °C and drain.
  • the fabric was given a reduction cleaning with Hydros and NaOH (1 gpl each), 90 °C for 20 min.
  • the fabric was then washed with cold water for 10 minutes, contacted with acetic acid (2 gpl) for 15 minutes, then washed with cold water for 10 minutes.
  • the fabric was then dyed with a mixture of acid dyes using the following time and temperature profile: heat to 70 °C and hold for 10 minutes, then raise temperature 1.5 °C/min to 98 °C and hold for 45 minutes, then decrease temperature 1.5 °C/min to 70 °C and drain.
  • the fabric was washed in cold water (10 minutes), treated with acetic acid (1 gpl for 15 minutes), subjected to a hot soaping with Albatex AD (90 °C for 15 minutes), washed with hot water (85 °C for 15 minutes), washed with cold water (10 minutes), then contacted with Levocol HCF (0.5 gpl) at 50 °C for 20 minutes to fix the dye.
  • the fabric was decatized in an autoclave (130 °C for 3 minutes) then padded with finishing agent before being heat set at 160 °C for 45 seconds in a lab stenter, and then decatized again in an autoclave (130 °C for 3 minutes).
  • Pellets of polytrimethylene terephthalate (PTT) containing 0.3% T1O2 and having an intrinsic viscosity of 0.96 dL/g and pellets of polyethylene terephthalate co-ethylene isophthalate (Co-PET) (from Nan Ya Plastics) having an intrinsic viscosity of 0.80 dL/g were dried separately at 120 °C under nitrogen blanket in a vacuum oven for 16 hours. Dried pellets of PTT and dried pellets of Co-PET were blended together in a small drum by hand shaking and rolling actions of the drum in the ratios give in Table 11.
  • Each of the salt-and-pepper blends thus created was melt-extruded into round cross-section, 34-filament yarn bundle using a twin-screw extruder spinning machine. Extruder melt zone temperatures were maintained from 180-265 °C. Polymer throughput, winder speed, spun denier per filament, and dry heat shrinkage of yarn bundles (tow) are provided in Table 11. Table 11. Example 25 Spinning Conditions and Dry Heat Shrinkage of Tow
  • a single-screw extruder was used to co-feed polytrimethylene
  • terephthalate and co-PET from Nan Ya Plastics a 7590-hole spinneret in 20:80 weight ratio.
  • Polytrimethylene terephthalate contained 0.3% T1O2 and had an intrinsic viscosity of 0.96 dL/g.
  • Round cross-section filaments were spun at an extruder throughput of 100 kg/h using radial quench. Extruder melt zone temperatures were maintained from 252-263 °C. Polymer throughput was 0.220 g/min/hole and feed roll speed was 650 m/m.
  • Spun dpf was nominally 3.4. Spun fibers were collected in cans.
  • Drawn tow was pulled through a steam chest at 100 °C by a downstream heated roll at 165 °C and running at 88.20 m/m. Tow was passed over another set of rolls heated at 165 °C running at 88.20 m/m. Finish (2% concentration, Duron 14 + Duron 1105 PE, 30/70 active substance, both by comp. CHT) was sprayed and tow was passed over cooling drum rolls at 25 °C, running at 86.44 m/m. Tow entered a steam box at 100 °C prior to entering a 40-mm crimper. Crimper speed was 90.76 m/m. Crimper roller temperature and pressure was 65 °C and 0.8 bar, respectively. Crimped tow was annealed for 4 min at 100 °C in a plate belt drier, Crimped tow was finally cut to produce staple melt spun fiber having the following properties (which were determined using the methods disclosed herein above):
  • a single-screw extruder was used to co-feed polytrimethylene
  • Drawn tow was pulled through a steam chest at 100 °C by a downstream heated roll at 165 °C and running at 92.22 m/m. Tow was passed over another set of rolls heated at 165 °C running at 90.38 m/m. Finish (2% concentration, Duron 14 + Duron 1105 PE, 30/70 active substance, both by comp. CHT) was sprayed and tow was passed over cooling drum rolls at 25 °C, running at 90.38 m/m. Tow entered a steam box at 100 °C prior to entering a 40-mm crimper. Crimper speed was 94.89 m/m. Crimper roller temperature and pressure was 65 °C and 0.8 bar, respectively. Crimped tow was annealed for 4 min at 100 °C in a plate belt drier, Crimped tow was finally cut to produce staple melt spun fiber having the following properties (which were determined using the methods disclosed herein above):
  • a single-screw extruder was used to co-feed polytrimethylene
  • a typical worsted count staple process utilizing multi-stage draw, crimper, annealer, and cutter was used to produce staple melt spun fiber.
  • Tow was dipped in a finish bath (0.5% concentration, commercially available, Duron 3176 from CHT) at 22 °C.
  • finish bath (0.5% concentration, commercially available, Duron 3176 from CHT) at 22 °C.
  • Tow was first drawn, in a 0.5% concentration finish bath at 75 °C between a 18 °C feed roll running at 30 m/m and heated draw rolls at 80 °C running at 114 m/m, giving a first stage draw ratio of 3.8.
  • Drawn tow was pulled through a steam chest at 100 °C by a downstream heated roll at 165 °C and running at 108.3 m/m.
  • Tow was passed over another set of rolls heated at 165 °C running at 106.1 m/m. Finish (2% concentration, Duron 14 + Duron 1105 PE, 30/70 active substance, both by comp. CHT) was sprayed and tow was passed over cooling drum rolls at 25 °C, running at 107.2 m/m. Tow entered a steam box at 100 °C prior to entering a 40-mm crimper. Crimper speed was 112.56 m/m. Crimper roller temperature and pressure was 65 °C and 0.8 bar,
  • Crimped tow was annealed for 4 min at 100 °C in a plate belt drier, Crimped tow was finally cut to produce multiple cut length staple melt spun fiber having the following properties (which were determined using the methods disclosed herein above):
  • Staple length multiple cut length, 59.5/79.3/119 mm
  • a single-screw extruder was used to co-feed CRASTIN® 6130C NC010 polybutylene terephthalate (PBT) having an intrinsic viscosity of 1.15 dL/g and co-PET (from Nan Ya Plastics) in 20:80 weight ratio through a 7590-hole spinneret. Round cross-section filaments were spun at an extruder throughput of 100 kg/h using radial quench. Extruder melt zone temperatures were maintained from 252-263 °C. Polymer throughput was 0.220 g/min/hole and feed roll speed was 650 m/m. Spun dpf was nominally 3.18. Spun fibers were collected in cans.
  • PBT polybutylene terephthalate
  • Drawn tow was pulled through a steam chest at 100 °C by a downstream heated roll at 165 °C and running at 92.61 m/m. Tow was passed over another set of rolls heated at 165 °C running at 92.61 m/m. Finish (2% concentration, Duron 14 + Duron 1105 PE, 30/70 active substance, both by comp. CHT) was sprayed and tow was passed over cooling drum rolls at 25 °C, running at 90.76 m/m. Tow entered a steam box at 100 °C prior to entering a 40-mm crimper. Crimper speed was 95.30 m/m. Crimper roller temperature and pressure was 65 °C and 0.8 bar, respectively. Crimped tow was annealed for 4 min at 100 °C in a plate belt drier, Crimped tow was finally cut to produce staple melt spun fiber having the following properties (which were determined using the methods disclosed herein above):
  • Staple length 40 mm
  • a single-screw extruder was used to co-feed CRASTIN® 6130C NC010 polybutylene terephthalate (PBT) having an intrinsic viscosity of 1.15 dL/g and co-PET (from Nan Ya Plastics) in 50:50 weight ratio through a 7590-hole spinneret. Round cross-section filaments were spun at an extruder throughput of 122.2 kg/h using radial quench. Extruder melt zone temperatures were
  • Drawn tow was pulled through a steam chest at 100 °C by a downstream heated roll at 165 °C and running at 94.93 m/m. Tow was passed over another set of rolls heated at 165 °C running at 94.93 m/m. Finish (2% concentration, Duron 14 + Duron 1105 PE, 30/70 active substance, both by comp. CHT) was sprayed and tow was passed over cooling drum rolls at 25 °C, running at 93.03 m/m. Tow entered a steam box at 100 °C prior to entering a 40-mm crimper. Crimper speed was 97.69 m/m. Crimper roller temperature and pressure was 65 °C and 0.8 bar, respectively. Crimped tow was annealed for 4 min at 100 °C in a plate belt drier, Crimped tow was finally cut to produce staple melt spun fiber having the following properties (which were determined using the methods disclosed herein above):
  • Spun yarn was prepared using melt spun staple fiber from Example 28 according to the procedure of Example 5 except with the following differences:
  • the linear density of the final sliver was 4.75 g/meter and the Unevenness % was 1.75.
  • the roving hank was 1.2 s Ne.
  • the twist multiplier/twist per inch was 3.6/22.6
  • the Traveler size was 4/0 M1 HO
  • the spindle speed was 16500 rpm.
  • the spun yarn was wound onto a cone at 1500 meters/m in. Properties of the spun yarn are given in Table 13. Properties of the spun yarns of this and the following Examples were determined using the methods disclosed herein above.
  • Spun yarn was prepared using melt spun staple fiber from Example 27 according to the procedure of Example 32. Properties of the spun yarn are given in Table 13.
  • Spun yarn was prepared using melt spun staple fiber from Example 31 according to the procedure of Example 32. Properties of the spun yarn are given in Table 13. Example 35
  • Spun yarn was prepared using melt spun staple fiber from Example 30 according to the procedure of Example 32. Properties of the spun yarn are given in Table 13.
  • Spun yarn was prepared using melt spun staple fiber from Example 28 and cotton (Shankar 6 variety Indian cotton commercially obtained from north Indian states).
  • the cotton staple had average length of 31 mm and linear density of 4.1 microgram/inch (1.6 microgram/cm).
  • the spun yarn was made according to the procedure of Example 32. Properties of the spun yarn are given in Table 13.
  • Spun yarn was prepared using melt spun staple fiber from Example 27 and cotton (Shankar 6 variety Indian cotton commercially obtained from north Indian states).
  • the cotton staple had average length of 31 mm and linear density of 4.1 microgram/inch (1.6 microgram/cm).
  • the spun yarn was made according to the procedure of Example 8. Properties of the spun yarn are given in Table 13.
  • Spun yarn was prepared using melt spun staple fiber from Example 31 and cotton (Shankar 6 variety Indian cotton commercially obtained from north Indian states).
  • the cotton staple had average length of 31 mm and linear density of 4.1 microgram/inch (1.6 microgram/cm).
  • the spun yarn was made according to the procedure of Example 8. Properties of the spun yarn are given in Table 13.
  • Spun yarn was prepared using melt spun staple fiber from Example 30 and cotton (Shankar 6 variety Indian cotton commercially obtained from north Indian states).
  • the cotton staple had average length of 31 mm and linear density of 4.1 microgram/inch (1.6 microgram/cm).
  • the spun yarn was made according to the procedure of Example 8. Properties of the spun yarn are given in Table 13.
  • Spun yarn was prepared using melt spun staple fiber from Example 28 and commercially-obtained Tencel® staple fiber (Lenzing).
  • the Tencel® staple had average length of 40 mm and denier of 1.2 D.
  • the spun yarn was made according to the procedure of Example 10. Properties of the spun yarn are given in Table 13.
  • Spun yarn was prepared using melt spun staple fiber from Example 27 and commercially-obtained Tencel® staple fiber (Lenzing).
  • the Tencel® staple had average length of 40 mm and denier of 1.2 D.
  • the spun yarn was made according to the procedure of Example 10. Properties of the spun yarn are given in Table 13.
  • Spun yarn was prepared using melt spun staple fiber from Example 31 and commercially-obtained Tencel® staple fiber (Lenzing).
  • the Tencel® staple had average length of 40 mm and denier of 1.2 D.
  • the spun yarn was made according to the procedure of Example 10. Properties of the spun yarn are given in Table 13.
  • Spun yarn was prepared using melt spun staple fiber from Example 30 and commercially-obtained Tencel® staple fiber (Lenzing).
  • the Tencel® staple had average length of 40 mm and denier of 1.2 D.
  • the spun yarn was made according to the procedure of Example 10. Properties of the spun yarn are given in Table 13.
  • Example 44
  • Spun yarn was made using the worsted spinning system, according to the following procedure.
  • melt spun staple fiber from Example 29 was used to prepare the spun yarn of Example 44.
  • the nominal count spun for the spun yarn was 2/68s Nm.
  • Boiling water shrinkage percent is higher for spun yarns incorporating salt-and-pepper PET/PTT 50:50 melt spun staple as compared to that of spun yarns incorporating compounded PET/PTT 50:50 melt spun staple. All other properties were found to be similar.
  • the spun yarns of Examples 32 through 44 were used to make woven fabrics as indicated in Table 14. Plain weave (1/1 ) shirting fabrics were made using the spun yarns disclosed herein as the warp and weft (fill) yarns. For each woven fabric, the same yarn was used in both the warp and the weft. Fabric evaluation results are presented in Tables 15 and 16. Results are reported for finished fabric unless otherwise noted. Fabric properties of this and the following Examples were determined using the methods disclosed herein above.
  • Spun yarn from Example 32 was used as the warp and as the weft to prepare a plain weave (1/1 ) shirting fabric.
  • the warp yarns were sized before beaming using a CCI single end sizing machine using Elvanol-T25 PVA sizing agent. Using a warper at 350 m/min, a final beam with 1680 ends, a width of 18 inches, and end lengths of 3.5 meters was prepared. With the following denting plan:
  • the greige fabric was desized on an RBE lab Jigger machine as follows.
  • the fabric sample was loaded into the jigger filled with water (2 L), NaOFI (2 gpl), and wetting agent;
  • Levocol CESR wetting agent
  • the fabric was run in the bath for 60 mins, then the bath was drained, refilled with fresh water, and the temperature of the bath was raised to 85 °C.
  • the fabric was hot water washed for 15 min, and the bath was drained. The bath was again filled with water and the fabric was run through it for 15 min (cold water wash).
  • the fabric was then dyed with a mixture of disperse dyes using the following time and temperature profile: heat to 70 °C and hold for 10 minutes, then raise temperature 1.5 °C/min to 130 °C and hold for 30 minutes, then decrease temperature 1.5 °C/.min to 70 °C and drain.
  • Post dyeing the fabric was given a reduction cleaning with Hydros and NaOH (2 gpl each), 90 °C for 20 min.
  • the fabric was then washed with cold water for 10 minutes, contacted with acetic acid (2 gpl) for 15 minutes, then washed with cold water for 10 minutes.
  • the dyed fabric was padded with finishing agent (softener), then heat set at 160 °C for 45 seconds in an RBE lab stenter.
  • Spun yarn from Example 36 was used as the warp and as the weft to prepare a plain weave shirting fabric according to the procedure of Example 45 but with the following exceptions.
  • the pick value was set at 58 picks / inch on the loom.
  • the greige fabric was desized and bleached in a Jigger machine, heat set in a stenter, then dyed with a mixture of disperse dyes, then additionally dyed with a reactive dye under cotton dyeing conditions. Fabric construction is shown in Table 14. Wicking test results were 100%. Other fabric properties are presented in Tables 15 and 16.
  • Spun yarn from Example 37 was used as the warp and as the weft to prepare a plain weave shirting fabric according to the procedure of Example 49 but with the following exceptions.
  • the greige fabric was desized and bleached in a Jigger machine, heat set in a stenter, then dyed with a mixture of disperse dyes, then additionally dyed with a reactive dye under cotton dyeing conditions. Fabric construction is shown in Table 14. Wicking test results were 100%. Other fabric properties are presented in Tables 15 and 16.
  • Spun yarn from Example 38 was used as the warp and as the weft to prepare a plain weave shirting fabric according to the procedure of Example 49 but with the following exceptions.
  • the greige fabric was desized and bleached in a Jigger machine, heat set in a stenter, then dyed with a mixture of disperse dyes, then additionally dyed with a reactive dye under cotton dyeing conditions. Fabric construction is shown in Table 14. Wicking test results were 100%. Other fabric properties are presented in Tables 15 and 16.
  • Spun yarn from Example 39 was used as the warp and as the weft to prepare a plain weave shirting fabric according to the procedure of Example 49 but with the following exceptions.
  • the greige fabric was desized and bleached in a Jigger machine, heat set in a stenter, then dyed with a mixture of disperse dyes, then additionally dyed with a reactive dye under cotton dyeing conditions.
  • Spun yarn from Example 40 was used as the warp and as the weft to prepare a plain weave shirting fabric according to the procedure of Example 49, except that no peroxide killer was used at the end of the bleaching step.
  • the pick value was set at 65 picks / inch on the loom.
  • Spun yarn from Example 34 was used as the warp and as the weft to prepare a suiting fabric of 2/1 twill construction.
  • the warp yarns were sized before beaming using a CCI single end sizing machine using Elvanol-T25 PVA sizing agent and a softener. Using a warper at 350 m/min, a final beam with 1518 ends, a width of 18 inches, and end lengths of 3.5 meters was prepared. With the following denting plan:
  • the greige fabric was desized in a Jigger machine using a procedure similar to that of Example 49, except that Albatex AD was used in conjunction with Levocol CESR.
  • the fabric was then subjected to a hot water wash (85 °C for 15 minutes), a cold water wash (15 minutes), a neutralization step with acetic acid (15 minutes), and another cold water wash (15 minutes).
  • the fabric was allowed to dry flat in atmospheric conditions, then heat set at 170 °C for 45 seconds.
  • the fabric was then dyed with a mixture of disperse dyes using the following time and temperature profile: heat to 70 °C and hold for 10 minutes, then raise temperature 1.5 °C/min to 130 °C and hold for 30 minutes, then decrease temperature 1.5 °C/.min to 70 °C and drain.
  • the fabric was given a reduction cleaning with Hydros and NaOH (1 gpl each), 90 °C for 20 min.
  • the fabric was then washed with cold water for 10 minutes, contacted with acetic acid (2 gpl) for 15 minutes, then washed with cold water for 10 minutes.
  • the fabric was then dyed with a mixture of acid dyes using the following time and temperature profile: heat to 70 °C and hold for 10 minutes, then raise temperature 1.5 °C/min to 98 °C and hold for 45 minutes, then decrease temperature 1.5 °C/min to 70 °C and drain.
  • the fabric was washed in cold water (10 minutes), treated with acetic acid (1 gpl for 15 minutes), subjected to a hot soaping with Albatex AD (90 °C for 15 minutes), washed with hot water (85 °C for 15 minutes), washed with cold water (10 minutes), then contacted with Levocol HCF (0.5 gpl) at 50 °C for 20 minutes to fix the dye.
  • the fabric was decatized in an autoclave (130 °C for 3 minutes) then padded with finishing agent, Levofin HYP-5gpl Levocol PNLI-1 Ogpl, before being heat set at 160 °C for 45 seconds in a lab stenter, and then decatized again in an autoclave (130 °C for 3 minutes).
  • Spun yarns from Examples 32, 33, 34, and 35 were each used to prepare circular knit fabrics on a Mesdan lab knitter.
  • the greige fabric was heat set in an RBE stenter at 160 °C for 45 seconds, then scoured in an HTHP Beaker dyeing machine using the following procedure.
  • the fabric was scoured at 90 °C for 60 minutes with NaOFI (2 gpl) and wetting agent Levocol CESR (5 gpl) added.
  • the fabric was washed at 85 °C for 15 minutes, then with cold water for 15 minutes, then with a neutralization solution containing acetic acid (1 gpl) for 15 minutes, followed by another cold water wash for 15 minutes.
  • the scoured fabrics were then dyed in the same machine with a mixture of disperse dyes using the following time and temperature profile: heat to 70 °C and hold for 10 minutes, then raise temperature 1.5 °C/min to 130 °C and hold for 30 minutes, then decrease temperature 1.5 °C/.min to 70 °C and drain.
  • Post dyeing the fabric was given a reduction cleaning with Flydros and NaOFI (2 gpl each), 90 °C for 20 min.
  • the fabric was then washed with cold water for 10 minutes, neutralized with acetic acid (2 gpl) for 15 minutes, then washed again with cold water for 10 minutes.
  • the dyed fabric was padded with finishing agent (softener), then heat set at 160 °C for 45 seconds in a lab stenter. Fabrics construction and testing results are presented in Tables 17 and 18. Wicking test results were 100% for all the fabrics
  • Spun yarns from Example 36, 37, 38, and 39 were each used to prepare circular knit fabrics on a Mesdan lab knitter following the procedure of Example 58, except that after dyeing with the disperse dyes, the fabric was dyed in the same machine with a reactive dye mixture to which salt (60 gpl) was added, using the following time and temperature profile: heat to 60 °C and hold for 30 minutes, then add soda ash (15 gpl) and hold for 30 minutes before draining.
  • salt 60 gpl
  • the fabric was then washed with cold water for 10 minutes, washed with acetic acid (1 gpl) for 15 minutes, then given a hot soaping with Albatex AD (2 gpl) during which the temperature was raised to 90 °C and held for 15 minutes.
  • the fabric was then washed with hot water (85 °C) for 15 minutes, and then with cold water for 10 minutes.
  • the dye was fixed with Levocol HCF (0.5 gpl) during which the temperature was raised to 50 °C and held for 20 minutes.
  • the dyed fabric was padded with finishing agent then heat set at 160 °C for 45 seconds in a lab stenter. Fabric construction and testing results are presented in Tables 17 and 18. Wicking test results were 100% for all the fabrics
  • Spun yarns from Example 40, 41 , 42, and 43 were each used to prepare circular knit fabrics on a Mesdan lab knitter following the procedure of Example 18, except with a different mixture of disperse dyes and a different mixture of reactive dyes and no peroxide killer was used at the end of the bleaching step. Fabric construction and testing results are presented in Tables 17 and 18.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Artificial Filaments (AREA)
  • Nonwoven Fabrics (AREA)
  • Knitting Of Fabric (AREA)
  • Woven Fabrics (AREA)

Abstract

L'invention concerne des filés comprenant une fibre discontinue filée à l'état fondu comprenant un premier polymère et un second polymère, le premier polymère comprenant du poly(triméthylène téréphtalate) ou du poly(téréphtalate de butylène)) et le second polymère comprenant du poly(téréphtalate d'éthylène) ou du Co-PET, le Co-PET étant un copolymère de poly(téréphtalate d'éthylène) comprenant un monomère d'acide isophtalique ; et le premier polymère comprenant du poly(triméthylène téréphtalate)) et le rapport en poids du poly(triméthylène téréphtalate) au second polymère étant situé dans la plage d'environ 80:20 à environ 10:90 ; ou le premier polymère comprenant du poly(téréphtalate de butylène)) et le rapport en poids du poly(téréphtalate de butylène) au second polymère étant situé dans la plage d'environ 90:10 à environ 10:90. Le filé peut en outre comprendre une seconde fibre discontinue telle que du coton ou de la laine. Le filé est utile dans la préparation de tissus ayant des propriétés avantageuses.
EP19746554.5A 2018-06-28 2019-06-26 Filé comprenant une fibre discontinue de polyester et tissu le comprenant Pending EP3814562A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US201862691066P 2018-06-28 2018-06-28
US201862747999P 2018-10-19 2018-10-19
PCT/US2019/039183 WO2020006043A1 (fr) 2018-06-28 2019-06-26 Filé comprenant une fibre discontinue de polyester et tissu le comprenant

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EP3814562A1 true EP3814562A1 (fr) 2021-05-05

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EP (1) EP3814562A1 (fr)
JP (1) JP2021529895A (fr)
KR (1) KR20210024618A (fr)
CN (1) CN112639183A (fr)
BR (1) BR112020026622A2 (fr)
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WO2022184789A1 (fr) * 2021-03-02 2022-09-09 Sanko Tekstil Isletmeleri San. Ve Tic. A.S. Tissu de protection

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TW202001018A (zh) 2020-01-01
KR20210024618A (ko) 2021-03-05
US20210164131A1 (en) 2021-06-03
CN112639183A (zh) 2021-04-09
JP2021529895A (ja) 2021-11-04
BR112020026622A2 (pt) 2021-03-30
WO2020006043A1 (fr) 2020-01-02

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