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CN104105823B - Comprise the fabric of poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) long filament - Google Patents

Comprise the fabric of poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) long filament Download PDF

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Publication number
CN104105823B
CN104105823B CN201180075129.3A CN201180075129A CN104105823B CN 104105823 B CN104105823 B CN 104105823B CN 201180075129 A CN201180075129 A CN 201180075129A CN 104105823 B CN104105823 B CN 104105823B
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CN
China
Prior art keywords
spinning
yarn
long filament
fabric
ptt
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Expired - Fee Related
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CN201180075129.3A
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Chinese (zh)
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CN104105823A (en
Inventor
W.D.巴特斯
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EIDP Inc
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EI Du Pont de Nemours and Co
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    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/50Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/283Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent 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
    • D01F6/92Monocomponent 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
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D13/00Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft
    • D03D13/008Woven fabrics characterised by the special disposition of the warp or weft threads, e.g. with curved weft threads, with discontinuous warp threads, with diagonal warp or weft characterised by weave density or surface weight
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2321/00Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D10B2321/12Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of cyclic compounds with one carbon-to-carbon double bond in the side chain
    • D10B2321/121Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of cyclic compounds with one carbon-to-carbon double bond in the side chain polystyrene
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2501/00Wearing apparel

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Woven Fabrics (AREA)
  • Multicomponent Fibers (AREA)

Abstract

Poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) the spin-drawing fiber of thin DENIER is characterised in that high DENIER uniformity coefficient. The invention also discloses a kind of for the method with the spinning speed all even and fine Denier yarns of preparation of 4000 to 6000m/min. Poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) fiber package described herein is containing the polystyrene disperseing 0.1 to 3 weight % within it. The present invention discloses fabric prepared therefrom in addition.

Description

Comprise the fabric of poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) long filament
Technical field
The present invention relates to the method for spinning poly (aromatic dicarboxylic acid 1,3-propylene glycol ester) fiber, gained fiber and their purposes.
Background technology
As the processbearing astrocyte polymkeric substance that can be used for yarn fabric, poly-(aromatic dicarboxylic acid 1, ammediol ester), especially poly-(terephthalic acid 1,3-propylene glycol ester) (also referred to as 3GT, Triexta or PTT) be recently subjected to a lot of concern. Ptt fiber has excellent physics and chemical property. By the silk (SDY) of partially oriented polyester yarn (POY) or spin-drawing, (PET) the continuous modification polyester yarn prepared that is mainly polyethylene terephthalate multiple yarn fabric purposes as knitting and Woven fabric and supatex fabric such as spunbond PET in there is commercial applications widely. Weaving term " yarn " refers to a branch of ultimate fibre. Such as, shirt and blouse are made up of yarn usually, and this yarn is made up of the tow of 30-40 threads.
The polyester yarn comprising PET and PTT yarn is prepared by so-called melt spinning process, and is stated to be " melt and spin ". Solution spinning is a kind of thus molten polymer and the method extruded by the hole in so-called spinning nozzle. In typical yarn fabric purposes, spinning nozzle has multiple hole, is generally 30-40, and each hole has the diameter of about 0.25mm. Thus extrude plurality of threads from single spinning nozzle. Merging those long filaments to form tow, it is called yarn.
Polyester yarn can arbitrarily and the yarn of other types combinationally use or do not combinationally use with them. Therefore, polyester yarn can form full fabric or form warp thread, weft yarn or parallel in Woven fabric; Or as one of two or more yarns in union yarn, such as, use cotton, wool, artificial silk, cellulose acetate, other polyester, spandex and/or their combination.
The United States Patent (USP) 6 of the people such as Fujimoto, 284,370 disclose the method for the preparation of 1-2dpfPTT fiber, wherein the first roller are heated to 30-80 DEG C, 2nd roller is heated to 100-160 DEG C, and the stretch ratio applied between the first roller and the 2nd roller is in the scope of 1.3-4. In 13 examples and 11 counter-examples, except a counter-example, Fujimoto never heats the first roller extremely higher than the temperature of 60 DEG C. In all examples, the first roll temperature is in the scope of 50-60 DEG C.
The United States Patent (USP) 7 of Ding, 785,507 disclose the method for the preparation of 2-3dpfPTT fiber, wherein lead silk by first and are heated to 85-160 DEG C, lead silk by the 2nd and it is heated to 125-195 DEG C, and the stretch ratio applied between the first roller and the 2nd roller is in the scope of 1.1-2.Ding proposes 75 DEG C first lead a temperature and cause too much thread breakage. Uster result is about 0.90-0.95%. In all examples, first to lead the temperature of silk be 90 DEG C or higher.
The United States Patent (USP) 6,287,688 of the people such as Howell describes the preparation of distortion PTT yarn, and this yarn shows the feel of the tensile property of raising, fluffy volume and improvement compared with PET yarn. The people such as Howell describe and prepare partially oriented PTT yarn with the spinning speed of 2600m/m at the most. By contrast, PET carries out molten spinning to be multiple times than the speed of this speed routinely. For cost reason, high expectations can with the speed spinning PTT yarn higher than 2600m/min.
The United States Patent (USP) 6,923,925 of the people such as Chang discloses the composition comprising PTT, and PTT comprises the polystyrene (PS) of about 2%, and it can be spun in the silk of spin-drawing by molten with the speed of 5000m/min at the most. The people such as Chang do not mention the DENIER uniformity coefficient (DenierCV) for the yarn so produced completely, and do not mention the temperature of the silk godet roller used for the preparation of spin-drawing yet.
Need the PTT spin-drawing filament yarn of low denier, its can with business can spinning speed carry out spinning, and there is enough DENIER uniformity coefficient to possess practicality in the purposes preparing high quality fabric and clothes.
Summary of the invention
In first aspect, providing package of the present invention is containing the long filament of composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, based on the polystyrene of total weight 0.1 to 3 weight % of the polymkeric substance in described composition, wherein said long filament is characterised in that≤Denier per filament of the 3 ,≤DENIER variation coefficient of 2.5% and the degree of birefringence of at least 0.055.
In an embodiment, poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) is poly-(terephthalic acid 1,3-propylene glycol ester).
On the other hand, the present invention is provided for being formed the method for novel spinning elongate filaments, described long filament is characterised in that≤Denier per filament of 3 and the DENIER variation coefficient of≤2.5, described method comprises the orifice extruded polymer melts by having cross section shape, it comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, based on the polystyrene of total weight 0.1 to the 3 weight % of described polymkeric substance, thus form continuous thread extrudate, quench this extrudate so that it is solidified into continuous filament yarn, the first driving roll being heated in 70 to 100 DEG C of temperature ranges reels this long filament and rotates with the first speed of rotation, then on the 2nd driving roll being heated in 100 to 130 DEG C of temperature ranges, reel this long filament and rotate with the 2nd speed of rotation, further, with the linear speed of at least 4,000 ms/min (m/min) by described winding filament on wind-up roll, wherein the ratio of the first speed of rotation and the 2nd speed of rotation is in the scope of 1.75 to 3, thus form spin-drawing long filament, and it has≤Denier per filament of 3 and the DENIER variation coefficient of≤2.5%.
In an embodiment, poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) is poly-(terephthalic acid 1,3-propylene glycol ester).
On the other hand, providing package of the present invention is containing the fabric of the long filament containing composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, based on the polystyrene of total weight 0.1 to 3 weight % of the polymkeric substance in described composition, wherein said long filament is characterised in that≤Denier per filament of the 3 ,≤DENIER variation coefficient of 2.5% and the degree of birefringence of at least 0.055.
In an embodiment, poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) is poly-(terephthalic acid 1,3-propylene glycol ester).
Accompanying drawing explanation
Fig. 1 is the schematic diagram of an embodiment to the spinning nozzle melting charging according to the present invention.
Fig. 2 is the schematic diagram of an embodiment of the fiber spinning process according to the present invention.
Fig. 3 illustrates the loom being suitable for manufacturing the Woven fabric of the present invention.
Fig. 4 is the schematic diagram of the spinning-drawing machine used in example.
Fig. 5 is experimental result picture, and it illustrates that first leads a temperature to the effect of the DENIER variation coefficient, and the result using spinning-drawing machine #2 to obtain and those results using spinning-drawing machine #1 to obtain is contrasted.
Embodiment
In one aspect, the present invention relates to the long filament comprising composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, based on the polystyrene of total weight 0.1 to 3 weight % of the polymkeric substance in described composition, wherein said long filament is characterised in that≤Denier per filament (dpf) of the 3 ,≤DENIER variation coefficient (DENIER CV) of 2.5% and the degree of birefringence of at least 0.055.
In an embodiment, poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) is poly-(terephthalic acid 1,3-propylene glycol ester).
In an embodiment, long filament is continuous filament yarn herein. In an alternative embodiment, long filament is short yarn long filament herein. In an embodiment, plurality of threads merges to form multifilament herein. Thus the multifilament formed is suitable for distortion, and be suitable for expecting the final utilization in those uses of fabric of thin Denier yarns wherein, such as shirt, blouse, woman style underwear, socks etc.
Herein multifilament can be used for by methods known in the art formed knitting, weave and supatex fabric.
In an alternative embodiment, long filament is also applicable to the structure of multiple nonwoven material herein. Long filament can be arranged in random or accurate random network to form thread supatex fabric herein. In another embodiment, thread supatex fabric comprises many basic literary composition continuous filament yarn strands. In another alternative embodiment, thread supatex fabric comprises single root continuous filament yarn strand. In an alternative embodiment, thread supatex fabric comprises the many short yarn long filaments prepared by this paper long filament. Thread supatex fabric for purposes of the present invention is supatex fabric, and wherein basic structural element is the single random or accurate random long filament fragment arranged, instead of multifilament yarn fragment.
On the other hand, the present invention is provided for being formed the method for novel spinning elongate filaments, described long filament is characterised in that≤Denier per filament of 3 and the DENIER variation coefficient of≤2.5%, described method comprises the orifice extruded polymer melts by having cross section shape, it comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, based on the polystyrene of total weight 0.1 to the 3 weight % of described polymkeric substance, thus form continuous thread extrudate, quench this extrudate so that it is solidified into continuous filament yarn, the first driving roll being heated in 70 to 100 DEG C of temperature ranges reels this long filament and rotates with the first speed of rotation, then on the 2nd driving roll being heated in 100 to 130 DEG C of temperature ranges, reel this long filament and rotate with the 2nd speed of rotation, further, with the linear speed of at least 4,000 ms/min (m/min) by described winding filament on wind-up roll,Wherein the ratio of the first speed of rotation and the 2nd speed of rotation is in the scope of 1.75 to 3.
As shown in example provided below, it is set as higher than 70 DEG C when leading silk by first, with 4, during the speed spinning of 000m/min or higher≤the yarn denier CV of 3dpf significantly lower than when leading silk by first and be set as commercial typical temperature 60 DEG C, with the DENIER CV of the analogous composition yarn of identical speed spinning.
Term " the DENIER variation coefficient " (DENIER CV) refers to the DENIER variation coefficient by measuring purchased from the UsterYarnEvenness tester of UsterTechnologies. So-called " Uster tester " is measured the DENIER along the continuous strand length direction of single root of fiber or yarn and is made a variation. DENIER CV is canonical statistics parameter, represents the value by obtaining divided by average denier with DENIER standard deviation, measures with Uster tester.
Except as otherwise noted, concentration weight percent represents in the present invention. Specifically, should understand and poly-(terephthalic acid 1, ammediol ester) or concentration of herein polystyrene that other poly-(aromatic dicarboxylic acid 1,3-propylene glycol esters) are blended be expressed as the polystyrene weight percent relative to the total polymer weight in composition.
Unless stated otherwise, when providing numerical range herein, it should be appreciated that the end points of its covering scope. It will be appreciated that numerical value has the precision of the number of significant figures provided as described in ASTME29-08. Such as, numeral 3 should understand the scope containing 2.5 to 3.4, and numeral 3.0 should understand the scope containing 2.95 to 3.04.
For purposes of the present invention, unless otherwise expressly specified, description will relate to and wherein gather those embodiments that (aromatic dicarboxylic acid 1,3-propylene glycol ester) is poly-(terephthalic acid 1,3-propylene glycol ester) (PTT). Assuming that extent of polymerization is identical, the present invention's expansion to the concentration be weight of reply time other poly-(aromatic dicarboxylic acid 1,3-propylene glycol esters) carries out adjusting being suitable for the difference of the special acrylate monomers unit molecular weight related to.
The homopolymer of polystyrene and PTT and multipolymer are all applicable to the present invention. For purposes of the present invention, term " multipolymer " should be understood and not only contains dipolymer, and contains terpolymer, tetrapolymer etc. Term " multipolymer " is interpreted as containing the monomer of any number condensed together. For practical purposes, major part patent application is limited to homopolymer, dipolymer and terpolymer.
In an embodiment, long filament comprises composition, and described composition comprises the polystyrene (PS) of PTT and 3 to the 0.1 weight % of 97 to 99.9 weight %. In another embodiment, long filament comprises composition, and described composition comprises other polyester of the PTT of 70 to 99.5 weight %, the PS of 3 to 0.5 weight % and optional 29.5 weight % at the most. In another embodiment, long filament comprises composition, and described composition comprises the PS of PTT and 2 to the 0.5 weight % of 98 to 99.5 weight %.
In an embodiment, long filament is made up of composition substantially, and described composition is made up of the polystyrene (PS) of PTT and 3 to the 0.1 weight % of 97 to 99.9 weight % substantially. In another embodiment, long filament is made up of composition substantially, and described composition is substantially by the PS of the PTT of 70 to 99.5 weight %, 3 to 0.5 weight % with optionally other polyester of 29.5 weight % form at the most. In another embodiment, long filament is made up of composition substantially, and described composition is made up of the PS of PTT and 2 to the 0.5 weight % of 98 to 99.5 weight % substantially.
Suitable PTT polymkeric substance is formed by the polycondensation of 1,3-propylene glycol and terephthalic acid or dimethyl terephthalate (DMT). The straight chain, ring-type and the branched aliphatic dicarboxylic acid that there is 4-12 carbon atom for being selected from one or more suitable comonomers of its copolymerization or ester (such as succinic acid, pentanedioic acid, hexanodioic acid, dodecanedioic acid and 1,4-cyclohexane dicarboxylic acid and their corresponding esters); Except terephthalic acid or ester and there is aromatic dicarboxylic acid or the ester (such as m-phthalic acid and 2,6-naphthalic acid) of 8-12 carbon atom; Have 2-8 carbon atom (except 1, outside ammediol) straight chain, ring-type and branched chain aliphatic diol, such as ethylene glycol, 1,2-propylene glycol, 1,4-butyleneglycol, 3-methyl isophthalic acid, 5-pentanediol, 2,2-dimethyl-1, ammediol, 2-methyl-1,3-propanediol and 1,4-cyclohexanediol; And there is aliphatic series and the aromatic oxide glycol of 4-10 carbon atom, two (2-hydroxyethyl) ether of such as Resorcinol or there is poly-(ether) ethylene glycol of the molecular weight lower than 460, comprise diethylidene ether ethylene glycol. Described comonomer usually exists with the content within the scope of 0.5-15 mole of % in PTT multipolymer, and can the content of 30 moles of % at the most exist.
Described PTT can comprise other selected comonomers of trace so that characteristic can not be had remarkable disadvantageous impact by them. These type of other comonomers comprise the such as content 5-sodium-sulfoisophthalic acid within the scope of 0.2 to 5 mole of %. Can mix very small amount of three sense comonomers such as trimellitic acid for viscosity controller. Described PTT can with other polymer blendings of at the most 30 moles of %. Example is by other glycol, as above-mentioned those, obtained polyester.
In an embodiment, described PTT comprises the trimethylene terephthalate repeat units of at least 85 moles of %. In another embodiment, described PTT comprises the trimethylene terephthalate repeat units of at least 90 moles of %. In another embodiment, described PTT comprises the trimethylene terephthalate repeat units of at least 98 moles of %. In another embodiment, described PTT comprises the trimethylene terephthalate repeat units of 100 moles of %.
In an embodiment, the intrinsic viscosity (IV) that suitable PTT is characterised in that in 0.70dl/g to 2.0dl/g scope. In another embodiment, the IV that suitable PTT is characterised in that in 0.80dl/g to 1.5dl/g scope. In another embodiment, the IV that suitable PTT is characterised in that in 0.90dl/g to 1.2dl/g scope.
In an embodiment, the number-average molecular weight (M that suitable PTT is characterised in that in 20,000Da to 25,000Da scopen). In another embodiment, the M that suitable PTT is characterised in that in 20,000Da to 25,000Da scopen
In an embodiment, the polystyrene being suitable for is selected from polystyrene homopolymer, Alpha-Methyl polystyrene and styrene-butadiene copolymer and their blend. In an embodiment, described polystyrene is polystyrene homopolymer. In another embodiment, the M that described polystyrene homopolymer is characterised in that in 5,000Da to 300,000Da scopen. In another embodiment, the M of polystyrene homopolymernIn the scope of 50,000Da to 200,000Da. In another embodiment, the M of polystyrene homopolymernIn the scope of 75,000Da to 200,000Da.In another embodiment, the M of polystyrene homopolymernIn the scope of 120,000Da to 150,000Da. Available polystyrene can be isotactic, atactic or syndiotaxy. High-molecular weight atactic polystyrene homopolymer is preferred.
Polystyrene used in the present invention can be commercially available from many suppliers, comprise DowChemicalCo. (Midland, Mich.), BASF (MountOlive, N.J.) and Sigma-Aldrich (SaintLouis, Mo.).
By PTT and PS melt blending, then extrude with strand form, it is cut into pellet subsequently. Also can carry out other forms of melt blending and pulverizing subsequently, as formed thin slice, fragment or powder. Can conveniently prepare the pellet comprising a PTT/PS blend and certain density PS (being greater than 15%) in some cases, melting pellet also dilutes melts to form the 2nd melt blended material with additional PTT again more subsequently, described 2nd melt blended material has≤the PS concentration of 3%, and the 2nd melt blended material is extruded and forms long filament herein.
Long filament comprises the composition containing PTT and PS herein. In certain embodiments, these will for bi-material only in blend and total is 100 weight % by they. But, blend will have other compositions in many cases, such as be generally comprised within polyester polymer composition for commercial use. Examples of such additives includes but not limited to other polymkeric substance, softening agent, UV light absorber, fire retardant, dyestuff etc. Therefore, total amount that is poly-(terephthalic acid 1,3-propylene glycol ester) and polystyrene will not be 100 weight %. Other polymkeric substance can comprise such as polymeric amide, and it gives union yarn can sour seven property. Under adding those situations of polymkeric substance additional, non-polyester wherein, polyester keeps identical with those compositions not comprising other polymkeric substance with the ratio of the weight percent concentration of PS.
According to the present invention, PS is particle form, and it has the mean sizes being less than 500 nanometers. In an embodiment, polystyrene is polystyrene homopolymer, and concentration is≤2%; And gather the PTT that (aromatic dicarboxylic acid 1,3-propylene glycol ester) is the propylene glycol ester terephthalate's monomer unit comprising at least 98 moles of %.
The long filament of the present invention is characterised in that≤dpf of 3 ,≤DENIER the CV and at least 0.055 of 2.5% degree of birefringence. The typical physical characteristic of long filament comprises the elongation at break of the toughness higher than 3 grams/DENIER and 30 to 70% herein. In an embodiment, long filament DENIER is≤2.5. In another embodiment, degree of birefringence is at least 0.060.
On the other hand, the present invention relates to the method for the preparation of monofilament or multifilament, described method comprises (a) and prepares the melt blended material being substantially made up of PTT and 0.1 to 3 weight % (wt%) polystyrene (PS), the PTT long filament that the polymer melt blend that the spinning of (b) solution is so prepared comprises dispersion PS to form one or more.
The long filament of the present invention is prepared into spin-drawing long filament-namely, the long filament being fully stretched in spinning technique by facility. The long filament after referring to quenching that stretches completely has been stretched to its limit elongation at break. Preferably, spinning comprises and extrudes blend polymer herein by one or more holes of spinning nozzle with the spinning speed of at least 4,000m/m. The spinning fibre accumulation rate that term " spinning speed " refers to such as on machinery wind-up roll.
The high birefringence rate of >=0.055 is the feature of long filament of the present invention, and it is the direct result applying the high drawing force in long filament in spin-drawing method.High birefringence rate is the basic skills distinguishing the partially oriented staple of spin-drawing long filament with tensile deformation subsequently.
Fig. 1 is the schematic diagram of an embodiment of the solution spinning-drawing machine being applicable to the present invention. Producing in continuous fusion polymerizer 1 see Fig. 1, PTT, it is transferred to reversion twin screw extruder 3 in molten form via transmission pipeline 2 from here, and this twin screw extruder is provided with mixing region. Simultaneously, the pellet comprising PS via weight loss feeder 4 or other pellet feeding manner chargings in satellite extruder 5, wherein pellet be melted and in molten form via transmission pipeline 6, the mixing region of twin screw extruder 3 or from it swim charging in twin screw extruder 3. Twin screw extruder is formed PTT/PS melt blended material. Gained melt blended material in the spinning block comprising spinning nozzle 8, extrudes one or more continuous filament yarn 9 by described spinning nozzle via transmission pipeline 7 charging.
Fig. 2 describes according to a kind of suitable structure of the present invention for solution spinning. 34 threads 22 (all 34 threads do not illustrate) are made to be extruded through hole spinning nozzle 21. Long filament is formed as yarn bundle by cooling zone 23, and by finishing composition application device 24. Cooling zone comprises air quenching district, its air under room temperature and 60% relative humidities with the velocity shock yarn bundle of 40 feet/min. Air quenching district can be designed for so-called horizontal air quenching, and wherein gas moves across yarn line, or is designed for so-called radial direction quenching, and wherein gas source is positioned at and merges in the middle of long filament, and flows radially outward with 360 °. Radial quenching is evenly and effective quenching method. After finishing composition application device 24, make yarn by being set to 60 to 100 DEG C, an embodiment is set to the first driving godet roller 25 (being also called feeding roller) and the separation roller of 70 to 100 DEG C. Make yarn the first godet roller be separated on roller winding 6 to 8 times. Yarn drives godet roller (being also called draw roll) from the first godet roller by being set to the 2nd of 110 to 130 DEG C the, and described 2nd driving godet roller is separated roller and connects with the 2nd. Make yarn the 2nd godet roller be separated on roller winding 6 to 8 times. Draw roll speed is 4000 to 6000m/min, and the ratio of draw roll speed and feeding roller speed is in the scope of 1.75 to 3. Yarn is from draw roll by the 3rd driving godet roller 27, and described 3rd driving godet roller connects at room temperature operation and the 3rd of the fast 1-2% of roller speed of velocity ratio the 2nd godet roller the separation roller. Yarn is reeled 6 to 10 times on roller the 3rd. Yarn from the 3rd to roller by staggered jet 28, then lead to mate the 3rd to the wind-up roll 29 of the operate that roller exports.
See Fig. 2, according to this paper method, quenching winding filament at least one times, but preferably reels repeatedly around the first godet roller so that the first godet roller applies drawing force in extruding long filament, causes it to be left behind before quenching; In the downstream of the first godet roller, winding filaments at least one times, but preferably reels repeatedly around the 2nd godet roller, the 2nd leads silk applying drawing force in this part long filament between the first godet roller and the 2nd godet roller in this way. In the embodiment shown in Figure 2, long filament is used as the 3rd godet roller of relax rolls from the 2nd godet roller guiding, and this roller runs with the speed of the speed height 1-2% than the 2nd (stretching) godet roller. Long filament is from the 3rd godet roller guiding wind-up roll. The speed of winding filaments on wind-up roll is described as spinning speed. In typical case is arranged, wind-up roll is the controlled wind-up roll of tension force.
According to the present invention, by the temperature that the first godet roller is heated within the scope of 70-100 DEG C, and the 2nd godet roller is heated to the temperature within the scope of 100-130 DEG C.First godet roller drives with the first speed of rotation; 2nd godet roller drives with the 2nd speed of rotation. Fall to according to the ratio (stretch ratio) of the present invention the 2nd speed of rotation and the first speed of rotation in the scope of 1.75 to 3.
In an embodiment, the various plurality of threads of the present invention are extruded through spinnert. Merge the long filament so extruded to form yarn. Usually by apply some stir, twisting or both are in the long filament extruded or spinning streamline, cause long filament to interweave, thus yarn kept together. The yarn so formed comprises plurality of threads, every threads is characterised in that≤dpf of 3 ,≤DENIER the CV and at least 0.055 of 2.5% degree of birefringence. In an embodiment, long filament DENIER is≤2.5. In another embodiment, degree of birefringence is at least 0.060. Typical yarn comprises 34,48,68 and 72 threads, but merges unrestricted to prepare the long filament number of yarn.
Yarn formed according to the present invention is not limited only to be made up of the plurality of threads according to the present invention, but also can contain other long filaments. Such as, yarn formed according to the present invention can comprise other polyester and polymeric amide, polyacrylic ester and it may be desirable to other long filaments of other these type of long filaments. Other long filaments can also be staple fibre.
That formed by spin-drawing method mentioned above, formed according to the present invention yarn is suitable for makes false twist texturized charging yarn, usually implements described false twist texturing and spins line shape aesthetic property to provide to continuous polycondensation fiber. Although there is polytype texturing machine, they are well known in the art, and deformation method comprises (a) provides the yarn package formed according to above-mentioned spinning technique; B () makes yarn from unwinding package; C () makes yarn end through friction twisting element or false twist spindle, (d) causes spindle to rotate, thus the yarn upstream causing rotary spindle is twisted, and makes upstream twisting untwisting in the downstream of rotary spindle, applies heat simultaneously; And described yarn is wound up in package by (e).
The present invention can improve the output of thin DENIER (≤3dpf) spin-drawing PTT yarn spinning. The long filament of the present invention and yarn thereof are prepared with the spinning speed than the maximum spinning speed high 30 to 70% that can reach with pure PTT. The elongation that gained yarn is characterised in that in the elongation and toughness 20% scope of PTT multifilament and toughness, this PTT multifilament and yarn of the present invention are only is not both it containing PS (and it must carry out spinning with about 3000m/min). Therefore, the yarn being substantially made up of long filament of the present invention can be used for multiple uses of fabric, only need to carry out small adjustment in the textile manufacturing machine used. Gained yarn is used in those that for not comprising PS and the condition of the PTT yarn prepared with 3000m/min is identical or prepares particularly textuered yarn, fabric and carpet under conditions of similarity.
In the long filament of the present invention, PTT is continuously phase or " matrix ", and PS is the discontinuous phase being scattered in described PTT matrix. In an embodiment, the PS particle being dispersed in PTT matrix is of a size of≤500nm. In another embodiment, the PS particle being dispersed in PTT matrix is of a size of≤200nm.
The favorable characteristics of the present invention comprises can with the ability of the thin DENIER of spinning speed spinning of 4000m/min or higher, high strength, hard spin-drawing PTT yarn. These favorable characteristics depend on the small grain size of PS and disperse the volume homogeneity of PS in PTT, and it depends on the applying of the melt blending of enough high-shears then.There is not the threshold value granularity that spinning properties and/or the physical property at this place's staple declines suddenly. On the contrary, along with PS granularity becomes big, performance is deteriorated gradually. In the size range of 500nm or bigger, DENIER CV becomes big gradually. Similarly, specific uniformity coefficient threshold value is not existed for the size distribution in PTT matrix. Dispersed homogeneous degree is more good, and gained spinning long filament will be more even. The valuable especially useful effect of of the present invention prepares spin-drawing yarn, it is characterised in that is less than the DENIER CV of 2.5%. Low denier CV is especially important in for the preparation of the thin Denier yarns of uses of fabric. It is enough to guarantee that granularity is less than the shearing force of 500nm and sufficiently high dispersed homogeneous degree unless the method being dispersed in PTT by PS is characterised in that, otherwise DENIER CV will for≤2.5% being very impossible.
Apply to depend on the rotating speed of hybrid element, the viscosity of melts and the melts residence time in mixing region in the shearing force value of melts. If shearing force is too low, then have that PS is not broken and the trend that cannot start, or there is the trend that PS agglomerates into size fast and be greater than the droplet of 500nm.
Melt-mixing method for interval and can carry out both continuously. Those commonly using in so-called high-shear mixer field as mixing in polymkeric substance are suitable. The example of the high-shear batch type device of suitable commercially available acquisition includes but not limited to Banbury mixer and Xi Labende mixing tank. The example of continuous high-shear mixer comprises coaxial rotating twin-screw extruder and Farrel continuously stirring device. Reversion twin screw extruder is also suitable. In general, suitable high-shear mixer is that can apply minimum in polymer melt is 50/s, it is preferable that those of 100/s shearing rate. After melt blending, can be granulated gained blend for rear feeding in spinning-drawing machine, or can by direct for melt blended material charging in spinning-drawing machine. Another available method is mixed polymer melts. An example of this kind of method by for providing PTT melt to the first column plate of twin screw extruder from successive polymerization device, and by PS melt from satellite extruder charging in the mixing region of twin screw extruder, thus forms melt blended material. In another approach, in charging before twin screw extruder carries out melt blending, it is dry mixed the polymkeric substance of non-melting by rolling.
From good fiber spinnability energy angle, the mean particle size being greater than 500nm is not preferred. In addition, even continuous yarn spinning along single end mode and end-to-end mode obviously all depends on the homogeneity that PS particle volume distributes. Although not by the restriction of the scope of the invention, by inference in the melt-processed of its reality, PS particle fusion is to form molten drop, and it is dispersed in melting PTT Medium Culture.
Temperature in melting agitator should higher than the fusing point of PTT and PS, but the lowest decomposition temperature lower than any composition. Concrete temperature will depend on the specific object of polymkeric substance used. In typical practice, melt temperature is in the scope of 200 DEG C to 270 DEG C.
In an embodiment, the PS concentration in PTT/PS blend pellet is in the scope of 0.5 to 1.5%.
As shown in fig. 1, and also it is generally like this with regard to polymer fiber melt spinning, polymer melt is fed to spinning nozzle via transmission pipeline. The melts transmitting pipeline by forcing machine input is disorderly.But, spinning nozzle charging is necessary for laminar flow, with by formation constant speed stream during multiple hole in spinning nozzle. Melting stream becomes laminar flow from turbulent flow in transmission pipeline.
Conventional equipment and the method for business widespread use can be used, it is achieved continuous yarn spinning. , it has been found that in order to the thin DENIER long filament of spinning 3dpf or lower, in fact the PS concentration of > 3% causes the mechanical property of so fiber of generation to reduce. It has been found that under 5%PS, thin DENIER long filament can not melt and spin at all.
Before melt spinning, it is preferable that blend polymer pellet is dried to moisture content < 30ppm, with hydrolytic deterioration during avoiding melt spinning. Any dry means known in the art are all satisfactory. In an embodiment, it may also be useful to closed loop heat air dryer. Usually, by PTT/PS blend dry 6h under 130 DEG C of dew points with <-40 DEG C. Thus the PTT/PS blend polymer of drying is melt-spun into fiber at 250-265 DEG C.
In typical melt spinning process, its embodiment is described in detail in hereinafter, by the blend polymer pellet charging of drying in forcing machine, described forcing machine is by pellet melting and gained melts is supplied volume pump, and the polymer flow of controlled-volume is delivered to the spin pack of heating by described volume pump via transmission pipeline. Pump must provide the pressure of 10-20MPa to force fluid by spin pack, and described spin pack comprises filtration medium (such as casting bed and filter sieve), to remove any particle being greater than several microns. By volume pump control by the mass flow rate of spinning nozzle. Bottom subassembly, polymkeric substance leaves via the multiple apertures in metal slab (spinning nozzle) and enters gas quenching region. Although hole number and dimension thereof can significantly change, but single orifice has the diameter within the scope of 0.2-0.4mm usually. Advantageously at 235 to 295 DEG C, it is preferable that realize spinning under the spinneret temperature of 250 to 290 DEG C.
It is tending towards in the scope of 1-5g/min by the exemplary traffic of this size hole. Adopt multiple orifice cross section shape, but circular cross section is the most common. Usually, the rotating roller system control line speed of the high degree of controlled of the long filament spun is screwed by it. Filament diameter is by flow and batches speed decision; And can't help orifice size determine.
By spinning, line kinetics determines the long filament characteristic thus prepared, especially region between spinneret exits and long filament solidification point, and described region is called as quenching region. Quenching region specific design, by the airflow rate of the injection long filament of still mobility on quenching long filament characteristic there is very big impact. Usually the horizontal flow quenching of use and radial both quenchings. After quenching or solidification, long filament to batch speed advance, the 100-200 of the speed that described speed is normally left from orifice is doubly. Therefore, spin line to occur to accelerate at a high speed (and stretching) after orifice penetrates. The amount of orientation being frozen into spinning long filament is directly involved in the stress levels of solidification point director's silk.
Thus obtained melt-spun filaments is collected in the way of meeting desired end-use. Such as, with regard to being intended to change into the long filament of staple fibre, many continuous filament yarns can be merged into tow, described tow is accumulated in so-called little tank. Being intended to usually be wound on yarn package with continuous form for the long filament being such as out of shape, described yarn package is arranged on the controlled wind-up roll of tension force. According to the present invention, accumulation rate is at least 4,000m/min.
By being generally known as false twist texturized method, by twisting, thermal-setting and untwisting, distortion will be given curling. These multifilament (also referred to as " tow ") comprise the long filament of the silk with spin-drawing (long filament is prepared) identical number by it. Therefore, they preferably comprise at least 10, and even more preferably at least 25 threads, and usually can comprise nearly 150 or more, preferably nearly 100, it is more preferable to ground is 80 threads nearly. Yarn has at least 1 usually, it is more preferable to ground at least 20, it is preferable that at least 50, it is more preferable to ground at the most 250, and at the most 1,500 total DENIER. Long filament is preferably at least 0.1dpf, it is more preferable to ground is 0.5dpf at least, it is more preferable to ground is 0.8dpf at least, and most preferably 3dpf at the most.
By PTT/PS-blend solution being spun to long filament at the temperature of 245 to 285 DEG C, long filament is quenched, the long filament of quenching is stretched, the crimped filament that will stretch, and described long filament is cut into staple fibre, obtained PTT staple fibre, it is preferable that described staple fibre has the length of 0.2 to 6 inch (0.5 to 15cm). a kind of preferred method comprises: (a) providing package is containing the blend polymer of PTT and 0.1 to 3%PS, b melt blended material solution is spun to long filament by () at the temperature of 245 to 285 DEG C, c () is quenched this long filament, d the long filament of quenching is stretched by (), e () uses machinery to crispatura machine, with the long filament of the curling stretching of crimpness of 8 to 30 curling/inch (3 to 12 curling/centimetre), f () makes curling long filament relax at the temperature of 50 to 120 DEG C, and (g) is by lax long filament cutting short-forming fiber, preferably there is the length of 0.2 to 6 inch (0.5 to 15cm). in a preferred embodiment of the method, the long filament of stretching before curling, is made to anneal at 85 to 115 DEG C. heated roller is preferably used to anneal under tension. in another preferred embodiment, the long filament of stretching is not annealed before crimping. staple fibre is for the preparation of weaving yarn and yarn fabric or supatex fabric, and can be used for fibrefill application and manufacture carpet.
Although the present invention mainly describes multifilament, it should be understood that preferred requirement as herein described is applicable to monofilament.
Long filament can be circular or have other shapes, such as octofoil, trilateral, rising sun shape (also referred to as " sol "), the ellipse having knuckle-tooth, trilobal, four flute profiles (also referred to as " four grooves "), the band shape having knuckle-tooth, band shape, radial etc. They can be solid, hollow or porous.
On the other hand, providing package of the present invention is containing the fabric of the long filament containing composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, based on the polystyrene of total weight 0.1 to 3 weight % of the polymkeric substance in described composition, wherein said long filament is characterised in that≤Denier per filament of the 3 ,≤DENIER variation coefficient of 2.5% and the degree of birefringence of at least 0.055. In an embodiment, poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) is poly-(terephthalic acid 1,3-propylene glycol ester).
In an embodiment, by endless tow resultant yarn, and fabric is Woven fabric. In an alternative embodiment, endless tow is become at least one yarn, and fabric is knit goods. In another embodiment, fabric is supatex fabric; In another embodiment, fabric is nonwoven fabric.
In a definition, supatex fabric is neither Woven fabric neither knitted fabrics. Weave and it is characterised in that with knitted structure by the interlocking yarn regular pattern interweaved (weaving) or the collar (knitting) is obtained.In both cases, regular pattern followed by yarn, they to another side and is returned from the side band of fabric, goes round and begins again. Formed by fabric self structure and weave or the integrity of knitted fabrics.
In supatex fabric, the most commonly, long filament is laid with random patterns, and combine via chemical or thermal means instead of mechanical means each other. The example of a commercially available acquisition of the non-woven fabric produced by this type of method is purchased from DuPontCompanySpunbond polyester. In some cases, by making layer of fibers lay with complex three-dimensional topology arrays, obtained non-woven fabric, described array does not relate to intertexture or the collar, and wherein fiber is not rotated from side another side, such as the United States Patent (USP) 6 people such as Popper, described in 579,815.
With the obtained Woven fabric of the many yarns at right angles interweaved each other. The yarn being parallel to fabric length direction is called " warp thread " and the yarn in this direction orthogonal is called " parallel " or " weft yarn ". Each warp thread is called one " end ". This is found in any fabric or clothes shop, by change the ad hoc fashion of interlaced yarns, yarn denier, yarn this in the ratio of the aesthetics of sense of touch and visual aspects, yarn density and warp thread and weft yarn, it is possible to reach huge change aesthetically. As general rule, the structure of Woven fabric gives certain rigidity to fabric; The stretching of Woven fabric is generally big less than knitted fabrics.
In the Woven fabric of the present invention, warp thread comprises yarn at least partially, it comprises the long filament containing composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, based on the polystyrene of total weight 0.1 to 3 weight % of the polymkeric substance in described composition, wherein said long filament is characterised in that≤Denier per filament of the 3 ,≤DENIER variation coefficient of 2.5% and the degree of birefringence of at least 0.055. In an embodiment, poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) is poly-(terephthalic acid 1,3-propylene glycol ester).
In an embodiment, warp thread and weft yarn all comprise yarn, and described yarn comprises long filament herein. In an embodiment, what warp thread comprised at least 40% number comprises the herein yarn of long filament and the cotton yarn of at least 40% number. In an embodiment, warp thread comprises the yarn comprising long filament of at least 80% number, and weft yarn comprises the cotton yarn of at least 80%. Generally, the actual demand of warp thread is being greater than weft yarn.
Loom manufactures Woven fabric, as they so modes always over several thousand. Although loom there occurs huge change, basic operation logic is identical. Fig. 3 a is with the schematic diagram of the loom embodiment shown in side-view. Place the warp beam 31 being made up of multiple (usual hundreds of) parallel end 32 as loom charging. Warp beam 31 is shown in Fig. 3 b with frontview. Be shown in Fig. 3 a is two band tool looms. Each band tool 34a and 34b is the framework keeping many (usually hundreds of) alleged " combining line ". See Fig. 3 c, illustrating the amplification frontview of band tool 34, it is the vertical line wherein with hole 312 that every root combines line 311. Arranging band tool to move up and down, one moves up, and other move down. Make a part of end 33a through the hole 312 in the comprehensive line 311 of upper band tool 34a, and make another part of end 33b through the hole in the comprehensive line of lower harness 34b, thus open the gap between end 33a and 33b. In shown type loom, shuttle 36 (is generally wood paddle-tumble) in a way not illustrated and drives, when band tool moves up and down, to move from side or to shuttle back and forth to another side.Shuttle carries weft yarn 37 bobbin, and described bobbin moves by unwinding during warp thread tip gap at shuttle. So-called " reed " or " press strip " 35 keep end at the framework of freely through a series of vertical line therebetween. Fig. 3 d illustrates the reed 35 describing vertical line 313 in frontview, and the spacing 314 that warp thread passes through. The thickness of vertical line 314 determines the spacing of the horizontal warp thread of fabric, thus determines its density. Reed is for shifting onto on the right side of diagram by the weft yarn just inserted, and arrangement forms fabric 38. Fabric is wound on fabric axle 310. Roller 39 is guide roller.
Warp beam winding is accurate operation, yarn package or the spool of number identical with required end number are wherein installed usually on so-called bobbin frame, and each end is delivered in warp beam by a series of accurate guider and tightening device, then the disposable winding of whole warp beam.
The ratio of pattern, warp thread and weft yarn of specifically interweaving determines the type of obtained Woven fabric. Basic pattern comprise flat knit, twill weave and satin weave. Other more unique weaving-patterns many are also known.
Knitting is by being overlapped mutually by one or more yarn and the method for obtained fabric. Knitted fabrics is tending towards having the stretching bigger than weaven goods and elasticity. Knitted fabrics wearing quality is tending towards lower than weaven goods. With regard to weaving, there is many knit pattern and knitting patterns. According to the present invention, in an embodiment, fabric is the knit goods comprising yarn herein, described yarn comprises the long filament containing composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, based on the polystyrene of total weight 0.1 to 3 weight % of the polymkeric substance in described composition, wherein said long filament is characterised in that≤Denier per filament of the 3 ,≤DENIER variation coefficient of 2.5% and the degree of birefringence of at least 0.055. In an embodiment, poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) is poly-(terephthalic acid 1,3-propylene glycol ester).
Also imagine the clothes sewed by the fabric of the present invention in the present invention. Clothes herein comprises the fabric containing yarn, described yarn comprises the long filament containing composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, based on the polystyrene of total weight 0.1 to 3 weight % of the polymkeric substance in described composition, wherein said long filament is characterised in that≤Denier per filament of the 3 ,≤DENIER variation coefficient of 2.5% and the degree of birefringence of at least 0.055. In an embodiment, poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) is poly-(terephthalic acid 1,3-propylene glycol ester).
Manufacturing clothes by fabric is the technology that non-Changshu is known. Comprising preparation pattern by fabric knitting clothes, usually prepared by paper material, or prepare with form of computers with regard to automation process, the pieces of fabric needed for measurement, described, to prepare required sheet, is then stitched together by cutting fabric according to described pattern. Clothes can make one or more patterns of fabric of the present invention specially. Alternatively, clothes is prepared by the fabric of the present invention and other fabrics combining one or more patterns.
The present invention is also described in following specific embodiment, but not by their restriction.
Example
Testing method
Intrinsic viscosity
Viscotek forced-flow viscometer Y900 (ViscorekCorporation, Houston, Tex.) is used to measure the intrinsic viscosity (IV) of PTT. According to ASTMD-5225-92 method, at 19 DEG C, the solvent mixture of trifluoroacetic acid and 50/50 weight % of methylene dichloride is formed the PTT solution of 0.4g/dl, and measures viscosity.The IV value that these record associates according to ASTMD4603-96, the IV value manually recorded in the phenol/1,1,2,2-tetrachloroethane of 60/40 weight %.
Number-average molecular weight
The number-average molecular weight of polystyrene is measured according to ASTMD5296-97. Same procedure is used for poly-(terephthalic acid 1,3-propylene glycol ester), the difference is that calibration standard be have 44,000 MwPoly-(ethylene glycol terephthalate) and hexafluoroisopropanol solvent.
Toughness and elongation at break
The physical property of long filament and yarn uses tensile tester 1122 type of InstronCorp. to measure. More specifically, elongation at break Eb and toughness are measured according to ASTMD-2256.
Spinning to-and-fro movement and spinning-drawing machine are on the impact of result
Fiber sprinning carries out in four independent to-and-fro movements. As detailed below, to-and-fro movement #1,3 and 4 carries out on spinning-drawing machine #2, and to-and-fro movement #2 carries out on spinning-drawing machine #1.
The result obtained from spinning-drawing machine #1 is dispersion, as shown in table 4 and fig. 5, and is not considered as reliable. Specifically, the limit that the DENIER variation coefficient is specified higher than the present invention, and seem the change of not temperature generation systems along with the first godet roller.
Fig. 5 is the schematic diagram that DENIER CV leads a temperature to first, be wherein obtained from to-and-fro movement 1,3 with 4 all data be incorporated in together with and draw diamond curve figure, and trilateral mapping must be used from the data of to-and-fro movement #2. As shown in following table 3-6, not all being obtained from wherein uses three reciprocating data points of spinning-drawing machine #2 to utilize identical spinning condition setting to obtain. But, as shown in Figure 5, rhombus must be shown as from the data of spinning-drawing machine #2, it shows a clear and definite trend, wherein first leads a temperature in the scope of about 75 to 85 DEG C, corresponding to minimum DENIER CV. The data of to-and-fro movement #2 are not observed similar trend.
The DENIER variation coefficient is measuring of short range DENIER variability, and it is the instruction of melt spinning process stability then. Melt spinning process may be unstable, because spinning component causes unstable. It also may be unstable, because machine is unstable. From Fig. 5, it is clear that the high DENIER CV produced in to-and-fro movement #2 in this case is the artifact of machine performance and design.
Spinning-drawing machine #1 is the spinning-drawing machine being placed in laboratory, is only provided with the most basic equipment to carry out solution spinning. Whether usually only use spinning-drawing machine #1 to obtain can by the most basic information of solution spinned fiber about Experimental composition. It uses in this paper to-and-fro movement #2, this is because regularly mixing-spinning-drawing machine #2 is unavailable on the date of the #2 that regularly moves back and forth. Spinning-drawing machine #2 is pilot scale factory spinning production line. Its condition may extend to the spinning production line of full-scale commercial size completely. This selects the spinning production line for the result difference showing feature of present invention.
Fig. 4 schematically shows spinning-drawing machine #2. Silo drying machine 41, the single screw extrusion machine 42 of gravity charging, has dry resin blend pellet. Directly charging is in the input of toothed gear pump 43 under stress in the output of single screw extrusion machine 42, and toothed gear pump is provided with overflow port 44. The output of toothed gear pump transmits, via short (several inches long), the spin pack 46 that pipeline 45 is supplied to six ends, wherein uses four ends. Four are spun the every root in line 47 (illustrating) and are extruded (not shown) from 36 hole spinning nozzle, and wherein each hole is characterised in that diameter is 0.27mm and length is the circular cross section of 0.50mm.Every root spins the horizontal flow quenching air zone 48 of line 47 by the about 1.75m of length, wherein ambient air flows to another side from the side spinning line in to-and-fro movement 1, and by the radial quenching air zone 48 of the about 1.75m of length, wherein ambient air in to-and-fro movement 3 and 4 around spin line radial flow to produce even evenly long filament. Therefore every root quenching spin linear contact lay forming roll 49, and add thermal conductance silk (feeding roller) 410 and corresponding first around first subsequently and be separated roller 411 and reel and spin line to keep 6-8 time and separate. Spin line to lead subsequently and the 2nd add thermal conductance silk (draw roll) 412 and be separated roller 413 with the 2nd of the 2nd correspondence, through staggered jet (not shown) and thus arrival wind-up roll 414. Being not shown in addition, every root is led silk and is encapsulated to keep temperature by hot case part. Forcing machine is provided with 3 heating zone and a head district in output.
Spinning-drawing machine #1 and spinning-drawing machine #2 is substantially the same for the layout described in Fig. 4. A difference is that the quenching vent-pipe in spinning-drawing machine #1 is much narrower than its corresponding section on spinning-drawing machine #2.
In all examples and comparative example, report four average results spinning line of spinning simultaneously under every set condition. Before preparation test sample, spinning-drawing machine is made to reach stable state by running about 45 minutes after setpoint conditions changes. When the composition change of polymkeric substance, clean spinning-drawing machine with the PTT not containing PS. When spinning nozzle changes, wash machine between spinning is tested.
The preparation of blend polymer
The PS sample (0.8 and 0.55 weight %) being prepared in PTT in 30mmT/S forcing machine by co-fed dry PTT and PS. With the amount shown in table 1, willSemi-DullPTT resin granular material (1.02IV, purchased from DuPontCompany (Wilmington, DE)) poly-(terephthalic acid 1,3-propylene glycol ester) and polystyrene (168MKG2, purchased from BASF) pellet mixes. Before use that PTT is dry in a vacuum furnace, with nitrogen purge 14 hours at 120 DEG C. By two kinds of weightless chargings of polymkeric substance difference in the 4th cylinder region of Werner&PfleidererZSK-30 reversion twin screw extruder. The feeding rate used illustrates with Pounds Per Hour (pph) in Table 1. Described forcing machine has the cylinder that diameter is 30mm, and described cylinder is made up of 13 cylinder regions alternately arranged with two kneading portion and three conveyor zones, and the L/D ratio that described forcing machine has is 32. Each cylinder region independently is heated. Region 1-4 is set to 25 DEG C, and region 5-13 is set to 210 DEG C, 3/16 " strand mould is also set to 210 DEG C. Also cylinder section 8 is applied vacuum. Table 1 also illustrates the composition of charging, output speed and melt temperature. Extrudate quenches after leaving mould immediately in water, then uses standard granulating equipment to be a granulated into 1/8 " pellet.
Table 1
Solution spinning
The solution spinning of fiber is carried out as mentioned below in four independent spinning to-and-fro movements. Table 2 illustrates the spinning parameter keeping constant in each to-and-fro movement.
To-and-fro movement #1-spinning-drawing machine #2
So melt compounded pellet dried overnight to water content in 140 DEG C of dry silos of the PTT/PS blend of preparation is reduced to < 50ppm. By in the single screw extrusion machine of the melt blended material gravity charging of drying in Fig. 4 spinning-drawing machine #2 mentioned above. Forcing machine setting point (DEG C) in the 1-3 of region is respectively 230/255/263. By toothed gear pump, forcing machine is exported melting charging in spin pack. Spin pack is provided with six spinning sites, and wherein four are provided with spinning nozzle, and each spinning nozzle has 36 holes, and each bore dia is 0.27mm and length is 0.5mm, and is circular cross section.So every root yarn of preparation is 75 DENIER 36 filament yarns. Being arranged on shown in table 3 of first godet roller. Note the 2nd godet roller is remained on 110 DEG C and 4500rpm. Quenching air is horizontal flow quenching, has the air velocity of 0.35cm/s.
The code followed is as follows: the 2nd godet roller (draw roll) is set as 4500m/min and 110 DEG C, and does not change between experiment periods. Then test with the first godet roller (feeding roller) being set in 60 DEG C, and change speed to determine to produce when regulating in elongation at break to the scope of 55-65% the stretch ratio of most high-tenacity. For blend polymer #2 (0.055%PS), it has been found that when elongation at break is within the scope of expectation (that is, feeding roller is set in 2150m/min), the stretch ratio of 2.09 causes the highest toughness. Then the other feeding roller temperature spinning with 85 and 110 DEG C is continued. Blend polymer #1 (0.8%PS) follows identical code; Finding when elongation at break is within the scope of expectation (that is, feeding roller speed=1900m/min), the stretch ratio of 2.37 causes the highest toughness.
Result is shown in Table 3
Table 3: the result of to-and-fro movement #1
To-and-fro movement #2-spinning-drawing machine #1
In PTT, the novel melting blend of 0.80 weight % is with blend #1 is identical above. So melt compounded pellet dried overnight to water content in 140 DEG C of dry silos of the PTT/PS blend of preparation is reduced to < 50ppm. By in the single screw extrusion machine of the melt blended material pellet gravity charging of drying in Fig. 4 spinning-drawing machine #1 mentioned above. Forcing machine setting point (DEG C) in the 1-3 of region is respectively 230/255/263. By toothed gear pump, forcing machine is exported melting charging in spin pack. Spin pack is provided with six spinning sites, and wherein four are provided with spinning nozzle, and each spinning nozzle has 36 holes, and each bore dia is 0.27mm and length is 0.5mm, and is circular cross section. So every root yarn of preparation is 75 DENIER 36 filament yarns. Being arranged on shown in table 4 of first godet roller. Note the 2nd godet roller is remained on 110 DEG C and 4500rpm. Quenching air is horizontal flow quenching, has the air velocity of 0.35cm/s.
The code followed is as follows: the 2nd godet roller (draw roll) is set as 4500m/min and 110 DEG C, and does not change between experiment periods. Then test with the first godet roller (feeding roller) being set in 60 DEG C, and change speed to determine to cause when regulating in elongation at break to the scope of 55-65% the stretch ratio of most high-tenacity. For blend polymer #1 (0.8%PS), ensuing: finding when elongation at break is within the scope of expectation (that is, first godet roller speed=1900m/min), the stretch ratio of 2.37 causes the highest toughness.
Example 5 and 6 spinneret hole of diameter 0.27mm is implemented. Example 7 and 8 spinneret hole of diameter 0.32mm is implemented. Other spinning conditions are shown in table 2 and table 4. Result is shown in Table 4.
To-and-fro movement #3-spinning-drawing machine #2
Be used in to-and-fro movement #2 use the same crowd of PS/PTT comprising 0.80 weight %PS.
Use as identical spinning-drawing machine method as described in to-and-fro movement #1 and setting carry out solution spinning above, the difference is that in these examples spinning 75 DENIER/36 filament yarn and to quench be radial quenching. Spinning condition is shown in table 3 and table 5. Again forcing machine heating zone is set as 230/255/263 DEG C respectively. Spinnerette diameters is 0.27mm.By flow control to 37.5g/min. Result is shown in Table 5.
To-and-fro movement #4--spinning-drawing machine #2
The 3rd blend being prepared in PTT 0.8%PS by the method identical with the method for blend #2 mentioned above.
Use as identical spinning-drawing machine method as described in to-and-fro movement #3 and setting carry out solution spinning above,
The difference is that spinning 75 DENIER/72 filament yarn in these examples. Spinning condition is shown in table 3 and table 6. Again forcing machine heating zone is set as 230/255/263 DEG C respectively. Spinnerette diameters is 0.27mm. By flow control to 37.5g/min, the difference is that being recorded in here in example 12 and example 13. Result is shown in table 6.

Claims (5)

1. comprise the fabric of spin-drawing long filament, described long filament comprises composition, described composition comprises and is dispersed in poly-(terephthalic acid 1, ammediol ester) in, based on the polystyrene of total polymer gauge 0.1 to the 3 weight % in described composition, wherein said long filament is characterised in that≤Denier per filament of the 3 ,≤DENIER variation coefficient of 3% and the degree of birefringence of at least 0.055.
2. fabric according to claim 1, wherein said composition comprise be dispersed in poly-(terephthalic acid 1,3-propylene glycol ester), based on the polystyrene of total polymer gauge 0.5 to the 2 weight % in described composition.
3. fabric according to claim 2, wherein said composition substantially by be dispersed in poly-(terephthalic acid 1,3-propylene glycol ester), form based on the polystyrene of total polymer gauge 0.5 to the 2 weight % in described composition.
4. fabric according to claim 1, wherein said fabric is Woven fabric.
5. clothes, comprises fabric according to claim 1.
CN201180075129.3A 2011-10-07 2011-10-07 Comprise the fabric of poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) long filament Expired - Fee Related CN104105823B (en)

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US5993712A (en) * 1997-02-25 1999-11-30 Lurgi Zimmer Aktiengesellschaft Process for the processing of polymer mixtures into filaments
US6284370B1 (en) 1997-11-26 2001-09-04 Asahi Kasei Kabushiki Kaisha Polyester fiber with excellent processability and process for producing the same
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