CN103917703A - Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom - Google Patents

Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom Download PDF

Info

Publication number
CN103917703A
CN103917703A CN201180074821.4A CN201180074821A CN103917703A CN 103917703 A CN103917703 A CN 103917703A CN 201180074821 A CN201180074821 A CN 201180074821A CN 103917703 A CN103917703 A CN 103917703A
Authority
CN
China
Prior art keywords
yarn
spinning
long filament
poly
ptt
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
CN201180074821.4A
Other languages
Chinese (zh)
Inventor
W.D.巴特斯
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.)
EIDP Inc
Original Assignee
EI Du Pont de Nemours and Co
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 EI Du Pont de Nemours and Co filed Critical EI Du Pont de Nemours and Co
Publication of CN103917703A publication Critical patent/CN103917703A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • D02G3/045—Blended or other yarns or threads containing components made from different materials all components being made from artificial or synthetic material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/298—Physical dimension

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)

Abstract

A fine denier poly(trimethylene arylate) spun drawn fiber is characterized by high denier uniformity. A process for preparing uniform fine denier yarns at spinning speeds of 4000 to 6000 m/min is further disclosed. The poly(trimethylene arylate) fiber hereof comprises 0.1 to 3% by weight of polystyrene dispersed therewithin. Fabrics prepared therefrom are also disclosed.

Description

Poly-(aromatic dicarboxylic acid 1,3-PD ester) fiber, preparation method and fabric prepared therefrom
Technical field
The present invention relates to method, gained fiber and their purposes for spinning poly (aromatic dicarboxylic acid 1,3-PD ester) (poly (trimethylene arylate)) fiber.
Background technology
Form polymer as the fiber that can be used for textiles, poly-(aromatic dicarboxylic acid 1, ammediol ester), especially poly-(terephthalic acid (TPA) 1,3-PD ester) (also referred to as 3GT, Triexta or PTT) be subjected to a lot of concerns recently.Ptt fiber has excellent physics and chemical property.By the silk (SDY) of partially oriented polyester yarn (POY) or spin-drawing, be mainly continuous texture polyester yarn prepared by polyethylene terephthalate (PET) and there is business application widely at multiple textiles purposes such as knitting and Woven fabric and supatex fabric in such as spunbond PET.Weaving term " yarn " refers to a branch of filament.For example, shirt and blouse are made up of yarn conventionally, and described yarn is made up of the tow of 30-40 threads.
The polyester yarn that comprises PET and PTT yarn is prepared by so-called melt spinning process, and is stated to be " melt-spun ".Melt spinning is a kind of molten polymer thus the method extruded by the hole in so-called spinning head.In typical textiles purposes, spinning head has multiple holes, is generally 30-40, and each hole has the diameter of about 0.25mm.Thereby extrude plurality of threads from single spinning head.Merge those long filaments to form tow, it is called yarn.
Polyester yarn can be arbitrarily and the yarn of other types be used in combination or be not used in combination with them.Therefore, polyester yarn can complete fabric or in Woven fabric, is formed warp thread, weft yarn or parallel; Or as one of two or more yarns in blended yarn, for example, use cotton, wool, artificial silk, acetate fiber, other polyester, spandex and/or their combination.
The people's such as Fujimoto United States Patent (USP) 6,284,370 disclose the method for the preparation of 1-2dpf ptt fiber, wherein the first roller are heated to 30-80 ℃, second roller is heated to 100-160 ℃, and the draw ratio applying between the first roller and second roller is in the scope of 1.3-4.In 13 examples and 11 counter-examples, except a counter-example, Fuiimoto never heats the first roller to the temperature higher than 60 ℃.In all examples, the first roll temperature is in the scope of 50-60 ℃.
The United States Patent (USP) 7 of Ding, 785,507 disclose the method for the preparation of 2-3dpf ptt fiber, wherein the first seal wire are heated to 85-160 ℃, the second seal wire is heated to 125-195 ℃, and the draw ratio applying between the first roller and second roller is in the scope of 1.1-2.The first seal wire temperature that Ding proposition is 75 ℃ causes too much thread breakage.Uster result is about 0.90-0.95%.In all examples, the temperature of the first seal wire is 90 ℃ or higher.
The people's such as Howell United States Patent (USP) 6,287,688 has been described the preparation of distortion PTT yarn, and this yarn shows the tensile property of raising, fluffy volume and the feel of improvement compared with PET yarn.The people such as Howell have described to prepare partially oriented PTT yarn up to the spinning speed of 2600m/m.By contrast, PET carries out melt-spun with the speed that is multiple times than this speed routinely.For cost reason, high expectations can be with the speed spinning PTT yarn higher than 2600m/min.
The people's such as Chang United States Patent (USP) 6,923,925 discloses the composition that comprises PTT, and described PTT comprises approximately 2% polystyrene (PS), and it can be entered in the silk of spin-drawing by melt-spun with the speed of 5000m/min at the most.The people such as Chang are the DENIER uniformity (Denier CV) of the not mentioned yarn for production like this completely, and the also temperature of the not mentioned silk godet roller used of preparing spin-drawing.
Need the PTT spin-drawing filament yarn of low denier, its can with business can with spinning speed carry out spinning, and there is enough DENIER uniformitys to possess practicality in the purposes of preparing high-quality fabric and clothes.
Summary of the invention
In first aspect, the invention provides the long filament that comprises composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer in composition, be wherein characterised in that≤3 Denier per filament of long filament ,≤2.5% the DENIER coefficient of variation and at least 0.055 birefringence.
In one embodiment, poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
On the other hand, the invention provides the method that is used to form novel spinning elongate filaments, be characterised in that≤3 Denier per filament of this long filament and≤2.5 the DENIER coefficient of variation, described method comprises the spinneret orifice extruded polymer fused mass by having shape of cross section, described polymer melt comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer, thereby form continuous thread extrudate, quench this extrudate so that it is solidified into continuous filament yarn, being heated to reel on 70 to 100 ℃ of first driven rollers in temperature range this long filament with the first rotary speed rotation, then being heated to reel on 100 to 130 ℃ of second driven rollers in temperature range this long filament with the second rotary speed rotation, and, with at least 4, the linear speed of 000 m/min (m/min) by described winding filament to wind-up roll, wherein the ratio of the first rotary speed and the second rotary speed is in 1.75 to 3 scope, thereby form spin-drawing long filament, its have≤Denier per filament of 3 and≤2.5% the DENIER coefficient of variation.
In one embodiment, poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
On the other hand, the invention provides the fabric that comprises the long filament that contains composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer in composition, wherein said long filament is characterised in that≤3 Denier per filament ,≤2.5% the DENIER coefficient of variation and at least 0.055 birefringence.
In one embodiment, poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
Accompanying drawing explanation
Fig. 1 is the schematic diagram to an embodiment of spinning head melting feed according to the present invention.
Fig. 2 is according to the schematic diagram of fiber spinning process of the present invention embodiment.
Fig. 3 illustrates the loom that is suitable for manufacturing Woven fabric of the present invention.
Fig. 4 is the schematic diagram of the spinning machine that uses in example.
Fig. 5 is experimental result picture, and it illustrates the effect of the first seal wire temperature to the DENIER coefficient of variation, and the result that uses spinning machine #2 to obtain and those results that use spinning machine #1 to obtain are contrasted.
The specific embodiment
In one aspect, the present invention relates to the long filament that comprises composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer in composition, be wherein characterised in that≤3 Denier per filament (dpf) of long filament ,≤2.5% the DENIER coefficient of variation (DENIER CV) and at least 0.055 birefringence.
In one embodiment, poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
In one embodiment, long filament is continuous filament yarn herein.In an alternative embodiment, long filament is short yarn long filament herein.In one embodiment, plurality of threads merges to form multifilament herein.Thereby the multifilament forming is suitable for distortion, and be suitable for expecting therein the final use in those textiles purposes of thin Denier yarns, for example shirt, blouse, lady's underwear, socks etc.
Herein multifilament can be used for by methods known in the art form 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 fiber web to form thread supatex fabric herein.In another embodiment, thread supatex fabric comprises how basic civilian continuous filament yarn strand.In another alternative embodiment, thread supatex fabric comprises single continuous filament yarn strand.In an alternative embodiment, thread supatex fabric comprises the many short yarn long filaments of being prepared by this paper long filament.Thread supatex fabric is for purposes of the present invention supatex fabric, and wherein basic structural detail is the single random or accurate random long filament fragment arranging, rather than multifilament textile fragment.
On the other hand, the invention provides the method that is used to form novel spinning elongate filaments, be characterised in that≤3 Denier per filament of described long filament and≤2.5% the DENIER coefficient of variation, described method comprises the spinneret orifice extruded polymer fused mass by having shape of cross section, described polymer melt comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer, thereby form continuous thread extrudate, quench this extrudate so that it is solidified into continuous filament yarn, being heated to reel on 70 to 100 ℃ of first driven rollers in temperature range this long filament with the first rotary speed rotation, then being heated to reel on 100 to 130 ℃ of second driven rollers in temperature range this long filament with the second rotary speed rotation, and, with at least 4, the linear speed of 000 m/min (m/min) by described winding filament to wind-up roll, wherein the ratio of the first rotary speed and the second rotary speed is in 1.75 to 3 scope.
As shown in example provided below, when the first seal wire is set as higher than 70 ℃, with 4, the yarn denier CV of 000m/min or higher speed spinning time≤3dpf is significantly lower than in the time being set as commercial typical temperature 60 C by the first seal wire, with the DENIER CV of the analogous composition yarn of identical speed spinning.
Term " the DENIER coefficient of variation " (DENIER CV) refers to the DENIER coefficient of variation of measuring by the Uster Yam Evenness tester purchased from Uster Technologies.So-called " Uster tester " measures the DENIER variation along the single continuous strand length direction of fiber or yarn.DENIER CV is canonical statistics parameter, represents to pass through with DENIER standard deviation the value divided by average DENIER acquisition, by Uster tester mensuration.
Except as otherwise noted, concentration represents with percentage by weight in the present invention.Particularly, should understand and poly-(terephthalic acid (TPA) 1, ammediol ester) or herein concentration of the polystyrene of other poly-(aromatic dicarboxylic acid 1,3-PD ester) blend be expressed as the polystyrene percentage by weight with respect to total polymer weight in composition.
Unless stated otherwise, in the time providing number range herein, should understand the end points of its covering scope.Should understand, the precision of the number of significant figures providing described in ASTM E29-08 is provided numerical value.For example, numeral 3 is interpreted as containing 2.5 to 3.4 scope, and numeral 3.0 is interpreted as containing 2.95 to 3.04 scope.
For purposes of the present invention, unless clearly stated in addition, it is poly-(terephthalic acid (TPA) 1,3-PD ester) those embodiment (PTT) that description will relate to wherein poly-(aromatic dicarboxylic acid 1,3-PD ester).Suppose that extent of polymerization is identical, the present invention tackles the difference of the special acrylate monomers unit molecular weight that concentration adjustment is by weight suitable for relating to while extending to other poly-(aromatic dicarboxylic acid 1,3-PD esters).
The homopolymers of polystyrene and PTT and copolymer are all applicable to the present invention.For purposes of the present invention, term " copolymer " is interpreted as not only containing dimer, and contains terpolymer, quadripolymer etc.Term " copolymer " is interpreted as containing the monomer of any number condensing together.For practical purposes, most of patent application is limited to homopolymers, dimer and terpolymer.
In one embodiment, long filament comprises composition, the polystyrene (PS) of the PTT that described composition comprises 97 to 99.9 % by weight and 3 to 0.1 % by weight.In another embodiment, long filament comprises composition, the PTT that described composition comprises 70 to 99.5 % by weight, the PS of 3 to 0.5 % by weight and optionally other polyester of 29.5 % by weight at the most.In another embodiment, long filament comprises composition, the PS of the PTT that described composition comprises 98 to 99.5 % by weight and 2 to 0.5 % by weight.
In one embodiment, long filament is made up of composition substantially, and described composition is made up of the PTT of 97 to 99.9 % by weight and the polystyrene (PS) of 3 to 0.1 % by weight substantially.In another embodiment, long filament is made up of composition substantially, described composition substantially by the PS of the PTT of 70 to 99.5 % by weight, 3 to 0.5 % by weight and optionally at the most other polyester of 29.5 % by weight form.In another embodiment, long filament is made up of composition substantially, and described composition is made up of the PTT of 98 to 99.5 % by weight and the PS of 2 to 0.5 % by weight substantially.
Suitable PTT polymer is formed by the polycondensation reaction of 1,3-PD and terephthalic acid (TPA) or dimethyl terephthalate (DMT).For example, for being selected from straight chain, ring-type and side chain aliphatic dicarboxylic acid or the ester (succinic acid, glutaric acid, adipic acid, dodecanedioic acid and Isosorbide-5-Nitrae-cyclohexane dicarboxylic acid and their corresponding esters) with 4-12 carbon atom with one or more suitable comonomers of its copolymerization; For example, except terephthalic acid (TPA) or ester and there is aromatic dicarboxylic acid or the ester (M-phthalic acid and NDA) of 8-12 carbon atom; What have 2-8 carbon atom (removes 1, outside ammediol) straight chain, ring-type and side chain aliphatic diol, for example ethylene glycol, 1,2-propylene glycol, BDO, 3-methyl isophthalic acid, 5-pentanediol, 2,2-dimethyl-1, ammediol, 2-methyl isophthalic acid, ammediol and Isosorbide-5-Nitrae-cyclohexanediol; And thering is aliphatic series and the aromatic oxide glycol of 4-10 carbon atom, two (2-ethoxy) ether of for example hydroquinones or have poly-(vinethene) ethylene glycol lower than 460 molecular weight, comprises diethylidene ether ethylene glycol.Described comonomer conventionally exists with the content within the scope of 0.5-15 % by mole in PTT copolymer, and can exist by the content up to 30 % by mole.
Other selected comonomer that described PTT can comprise trace makes them can not have remarkable adverse influence to characteristic.These type of other comonomers comprise for example 5-sodium-sulfoisophthalic acid of content within the scope of 0.2 to 5 % by mole.Can mix very small amount of trifunctional comonomer for example trimellitic acid for viscosity control.Described PTT can with other polyblend of 30 % by mole at the most.Example is by other glycol, as above-mentioned those, the polyester making.
In one embodiment, the trimethylene terephthalate repeat units that described PTT comprises at least 85 % by mole.In another embodiment, the trimethylene terephthalate repeat units that described PTT comprises at least 90 % by mole.In another embodiment, the trimethylene terephthalate repeat units that described PTT comprises at least 98 % by mole.In another embodiment, the trimethylene terephthalate repeat units that described PTT comprises 100 % by mole.
In one embodiment, suitable PTT is characterised in that the intrinsic viscosity (IV) within the scope of 0.70 to 2.0dl/g.In another embodiment, suitable PTT is characterised in that the IV within the scope of 0.80 to 1.5dl/g.In another embodiment, suitable PTT is characterised in that the IV within the scope of 0.90 to 1.2dl/g.
In one embodiment, suitable PTT is characterised in that 10,000Da to 40, the number-average molecular weight (M within the scope of 000Da n).In another embodiment, suitable PTT is characterised in that 20,000Da to 25, the M within the scope of 000Da n.
In one embodiment, applicable polystyrene is selected from polystyrene homopolymer, Alpha-Methyl polystyrene and Styrene-Butadiene and their blend.In one embodiment, described polystyrene is polystyrene homopolymer.In another embodiment, described polystyrene homopolymer is characterised in that 5,000Da to 300, the Mn within the scope of 000Da.In another embodiment, the Mn of polystyrene homopolymer is 50, and 000Da to 200, within the scope of 000Da.In another embodiment, the Mn of polystyrene homopolymer is 75, and 000Da to 200, within the scope of 000Da.In another embodiment, the Mn of polystyrene homopolymer is 120, and 000Da to 150, within the scope of 000Da.Available polystyrene can be isotactic, atactic or syndyotactic.High-molecular weight atactic polystyrene homopolymer is preferred.
Can be used for polystyrene of the present invention can be commercially available from many suppliers, comprise Dow Chemical Co. (Midland, Mich.), BASF (Mount Olive, N.J.) and Sigma-Aldrich (Saint Louis, Mo.).
By PTT and PS melt blending, then extrude with strand form, be cut into subsequently pellet.Also can carry out the melt blending of other form and pulverizing subsequently, such as forming thin slice, fragment or powder.Can prepare easily in some cases the pellet that comprises a PTT/PS blend and certain density PS (being greater than 15%), melting pellet also dilutes melting again to form the second melt blended material with additional PTT more subsequently, described the second melt blended material has≤3% PS concentration, and the second melt blended material is extruded and formed long filament herein.
Long filament comprises the composition that contains PTT and PS herein.In certain embodiments, these will will add up to 100 % by weight for only bi-material in blend and they.But blend will have other compositions in many cases, such as in the polyester polymer composition being generally comprised within commercial use.Examples of such additives includes but not limited to other polymer, plasticizer, ultra-violet absorber, fire retardant, dyestuff etc.Therefore, the total amount of poly-(terephthalic acid (TPA) 1,3-PD ester) and polystyrene will not be 100 % by weight.Other polymer can comprise for example polyamide, and it gives blended yarn theobromine metachromia.Add therein in those situations of polymer additional, non-polyester, it is identical with those compositions that do not comprise other polymer that the ratio of the weight percent concentration of polyester to PS keeps.
According to the present invention, PS is particle form, and it has the average-size that is less than 500 nanometers.In one embodiment, polystyrene is polystyrene homopolymer, and concentration is≤2%; And poly-(aromatic dicarboxylic acid 1,3-PD ester) is the PTT of propylene glycol ester terephthalate's monomeric unit of comprising at least 98 % by mole.
Long filament of the present invention is characterised in that≤3 dpf ,≤2.5% DENIER CV and at least 0.055 birefringence.The typical physical characteristic of long filament comprises higher than the toughness of 3 grams/DENIER and 30 to 70% elongation at break herein.In one embodiment, long filament DENIER is≤2.5.In another embodiment, 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 that (a) prepares the melt blended material being substantially made up of PTT and 0.1 to 3 % by weight (wt%) polystyrene (PS), and the polymer melting blend that (b) melt spinning is so prepared comprises to form one or more PTT long filament that disperses PS.
Long filament of the present invention is prepared into spin-drawing long filament-, the long filament having been stretched completely in spinning technique expediently.Completely stretch and refer to that the long filament after quenching has been stretched to its limit elongation at break.Preferably, spinning comprises with at least 4, and the spinning speed of 000m/m is extruded blend polymer herein by one or more holes of spinning head.Term " spinning speed " refers to for example spinning fibre accumulation rate on mechanical wind-up roll.
>=0.055 high birefringence rate is the feature of long filament of the present invention, and it is the direct result that puts on the high tensile force of long filament in spin-drawing method.High birefringence rate is the basic skills of distinguishing the partially oriented staple fibre yarn of spin-drawing long filament and stretcher strain subsequently.
Fig. 1 is the schematic diagram that is applicable to an embodiment of melt spinning machine of the present invention.Referring to Fig. 1, PTT produces in continuous fusion polymerizer 1, and it is transferred to reversion double screw extruder 3 via transfer line 2 with melting form from here, and this double screw extruder is provided with Mixed Zone.Simultaneously, the pellet that comprises PS is via weightless feeding machine 4 or other pellet feed-type feeding satellite extruder 5, wherein pellet be melted and with melting form via transfer line 6, in the Mixed Zone of double screw extruder 3 or from it trip feeding double screw extruder 3.In double screw extruder, form PTT/PS melt blended material.Gained melt blended material comprises the spinning block of spinning head 8 via transfer line 7 feedings, extrude one or more continuous filament yarn 9 by described spinning head.
Fig. 2 has described according to the present invention for a kind of suitable structure of melt spinning.34 threads 22 (all 34 threads are not shown) are extruded by hole spinning head 21.Long filament is formed as yarn bundle by cooling zone 23, and by finishing agent application device 24.Cooling zone comprises air hardening district, wherein air under room temperature and 60% relative humidity condition with the velocity shock yarn bundle of 40 feet per minute clocks.Air hardening district can be designed for so-called horizontal air hardening, and wherein gas is moving across yarn line, or is designed for so-called radially quenching, and wherein source of the gas is positioned at and merges in the middle of long filament, and outwards flows fast with 360 °.Radially quenching is more equal even effective process for quenching.After finishing agent application device 24, make yarn by being made as 60 to 100 ℃, be made as in one embodiment first driving godet roller 25 (being also called feeding roller) and the separate roller of 70 to 100 ℃.Yarn is reeled 6 to 8 times around the first godet roller and separate roller.Yarn leads to the second driving godet roller (being also called draw roll) that is made as 110 to 130 ℃ from the first godet roller, described second drives godet roller to connect with the second separate roller.Yarn is reeled 6 to 8 times around the second godet roller and separate roller.Draw roll speed is 4000 to 6000m/min, and the ratio of draw roll speed and feeding roller speed is in 1.75 to 3 scope.Yarn drives godet roller 27 from draw roll by the 3rd, and the described the 3rd drives godet roller to connect the 3rd separate roller of the fast 1-2% of roller speed of at room temperature operation and velocity ratio the second godet roller.Yarn is reeled 6 to 10 times around the 3rd pair roller.Yarn by staggered jet 28, then leads to the wind-up roll 29 of the speed running of mating the 3rd pair roller output from the 3rd pair roller.
Referring to Fig. 2, according to this paper method, quenching winding filament at least one times, is still preferably reeled repeatedly around the first godet roller, makes the first godet roller apply tensile force in extruding long filament, causes it before quenching, to be left behind; In the downstream of the first godet roller, winding filaments at least one times, is still preferably reeled repeatedly around the second godet roller, and the second seal wire applies tensile force in the long filament part between the first godet roller and the second godet roller in this way.In the embodiment shown in Figure 2, long filament is the 3rd godet roller as relax rolls from the second godet roller guiding, and described the 3rd godet roller is with the speed operation than the high 1-2% of speed of second (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 to spinning speed.In typical case arranges, wind-up roll is the wind-up roll of tension force control.
According to the present invention, the first godet roller is heated to the temperature within the scope of 70-100 ℃, and the second godet roller is heated to the temperature within the scope of 100-130 ℃.The first godet roller drives with the first rotary speed; The second godet roller drives with the second rotary speed.According to the present invention, the ratio (draw ratio) of the second rotary speed and the first rotary speed drops in 1.75 to 3 scope.
In one embodiment, various plurality of threads of the present invention are extruded and passed through multi-holed jet.Merge the long filament of so extruding to form yarn.Conventionally by apply some stir, twisting or both in the long filament of extruding or spinning streamline, cause long filament to interweave, thereby yarn kept together.The yarn so forming comprises plurality of threads, and every threads is characterised in that≤3 dpf ,≤2.5% DENIER CV and at least 0.055 birefringence.In one embodiment, long filament DENIER is≤2.5.In another embodiment, birefringence is at least 0.060.Typical yarn comprises 34,48,68 and 72 threads, but it is unrestricted to merge long filament number to prepare yarn.
Yarn formed according to the present invention is not limited only to be made up of plurality of threads according to the present invention, but also can contain other long filaments.For example, yarn formed according to the present invention can comprise other polyester and polyamide, polyacrylate and other long filaments of other these type of long filaments that may expect.Other long filaments can be also staple fibre.
Can be by spin-drawing method mentioned above yarn that form, formed according to the present invention be suitable for and make false twist texturized feed yarn, conventionally implement described false twist texturing and spin line shape aesthetic property to provide to continuous polycondensation fiber.Although have polytype texturing machine, they are well known in the art, deformation method comprises that (a) provides the yarn package forming according to spinning process mentioned above; (b) make yarn unwinding from package; (c) make yarn end through friction twisting element or false twist spindle, (d) cause spindle rotation, thereby cause the yarn upstream twisting of rotary spindle, and make upstream twisting untwisting in the downstream of rotary spindle, apply heat simultaneously; And (e) described yarn is wound up in package.
The present invention can improve the output of thin DENIER (≤3dpf) spin-drawing PTT yarn.Long filament of the present invention and yarn thereof are with than being prepared with high 30 to 70% the spinning speed of the accessible maximum spinning speed of pure PTT.Gained yarn is characterised in that percentage elongation and the toughness in the percentage elongation of PTT multifilament and toughness 20% scope, and this PTT multifilament and yarn of the present invention be only not to be both it and not to contain 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 textiles purposes, only need in the textiles machine using, carry out small adjustment.Gained yarn is used under or conditions of similarity identical with those conditions for the PTT yarn that do not comprise PS and prepare with 3000m/min prepares particularly textured yarn, fabric and carpet.
In long filament of the present invention, PTT is continuous phase or " matrix ", and PS is the discontinuous phase being scattered in described PTT matrix.In one embodiment, be dispersed in the be of a size of≤500nm of PS particle in PTT matrix.In another embodiment, be dispersed in the be of a size of≤200mn of PS particle in PTT matrix.
Favorable characteristics of the present invention comprises can be with 4000m/min or the higher thin DENIER of spinning speed spinning, high strength, hard spin-drawing PTT yarn.These favorable characteristics depend on the small grain size of PS and in PTT, disperse the volume uniformity of PS, and it depends on the melt blending that applies enough high shears then.There is not the threshold value granularity declining suddenly in spinning properties and/or the physical characteristic of this place's staple fibre yarn.On the contrary, along with PS granularity becomes large, performance is variation gradually.In 500nm or larger particle size range, it is large that DENIER CV becomes gradually.Similarly, there is not specific uniformity threshold value for the distribution of particles in PTT matrix.Dispersed homogeneous degree is better, and gained spinning long filament will be more even.A valuable especially beneficial effect of the present invention is to prepare spin-drawing yarn, it is characterized in that being less than 2.5% DENIER CV.Low denier CV is even more important in the preparation of the thin Denier yarns for textiles purposes.Unless the method characteristic that PS is dispersed in PTT is that sufficient to guarantee granularity is less than shearing force and the sufficiently high dispersed homogeneous degree of 500nm, otherwise DENIER CV will be the≤2.5%, very impossible.
The shearing force value that puts on fused mass depends on the viscosity of the rotating speed of hybrid element, fused mass and the fused mass time of staying in Mixed Zone.If shearing force is too low, there is the not broken and trend that cannot start of PS, or exist PS to agglomerate into fast the trend that size is greater than the droplet of 500nm.
Melt-mixing method can be for intermittently and continuously carrying out both.Those that commonly use in the mixing field of so-called high-shear mixer such as polymer are suitable.The example of the high shear batch agitator of suitable commercially available acquisition includes but not limited to Banbury mixer and Xi La Bender blender.The example of high-shear mixer comprises coaxial rotation double screw extruder and Farrel continuous stirred tank reactor continuously.Reversion double screw extruder is also suitable.In general, suitable high-shear mixer is that can in polymer melt, apply minimum is 50/s, those of preferred 100/s shear rate.After melt blending, can granulation gained blend for feed subsequently in spinning machine, or can be by direct melt blended material feed in spinning machine.Another available method is mixed polymer fused mass.An example of this method is for first column plate of PTT melt to double screw extruder is provided from continuous polymerization device, and by PS melt the Mixed Zone from satellite extruder feeding double screw extruder, thereby form melt blended material.In another approach, before double screw extruder carries out melt blending, can be dry mixed by rolling the polymer of not melting at feed.
From good fibre spinning performance perspective, the particle mean size that is greater than 500nm is not preferred.In addition, obviously all depend on along the even continuous yarn spinning of single end mode and end to end system the uniformity that PS particle volume distributes.Although be not subject to the restriction of the scope of the invention, in its actual melt-processed, PS particle fusion is to form molten drop by inference, and it is dispersed in melting PTT matrix.
Temperature in melting agitator should be higher than the fusing point of PTT and PS, but lower than the lowest decomposition temperature of any composition.Concrete temperature will depend on the specific object of polymer used.In typical practice, melt temperature is in the scope of 200 ℃ to 270 ℃.
In one embodiment, the PS concentration in PTT/PS blend pellet is in 0.5 to 1.5% scope.
As shown in fig. 1, and with regard to polymer fiber melt spinning, be also generally so, polymer melt is fed into spinning head via transfer line.Fused mass by extruder input transfer line is disorderly.But spinning head feed is necessary for laminar flow, during with multiple hole in by spinning head, form uniform flow.Melt-flow becomes laminar flow from turbulent flow in transfer line.
Conventional equipment and the method that can use business extensive use, realize continuous yarn spinning.In fact, find for spinning 3dpf or lower thin DENIER long filament, the PS concentration of > 3% causes the mechanical performance of the fiber so producing to reduce.Also find, under 5%PS, thin DENIER long filament at all can not melt-spun.
Before melt spinning, preferably blend polymer pellet is dried to moisture < 30ppm, to avoid hydrolytic degradation during melt spinning.Any dry means known in the art are all satisfactory.In one embodiment, use closed loop heat air dryer.Conventionally, by PTT/PS blend dry 6h under the dew point of mono-40 ℃ of 130 ℃ and <.Thereby dry PTT/PS blend polymer is melt-spun into fiber at 250-265 ℃.
In typical melt spinning process, an one embodiment describes in detail below, by dry blend polymer pellet feeding extruder, described extruder is supplied with measuring pump by pellet melting and by gained fused mass, and described measuring pump is delivered to the polymer flow of volume control the filament spinning component of heating via transfer line.Pump must provide the pressure of 10-20MPa to force fluid to pass through filament spinning component, and described filament spinning component comprises filter medium (for example casting bed and sieves), to remove any particle that is greater than several microns.By measuring pump control by the mass flow of spinning head.In assembly bottom, polymer leaves and enters gas quenching region via the multiple apertures in metal thick plate (spinning head).Although number of perforations and dimension thereof can significantly change, single spinneret orifice has the diameter within the scope of 0.2-0.4mm conventionally.Advantageously, at 235 to 295 ℃, preferably at the spinning head temperature of 250 to 290 ℃, complete spinning.
Be tending towards in the scope of 1-5g/min by the exemplary traffic of this size hole.Spinneret orifice adopts multiple shape of cross section, but circular cross section is modal.Conventionally, by its screw spin the rotating roller system control line speed of height control of long filament.Filament diameter is determined by flow and infiltration rate; And can't help spinneret orifice size determine.
The long filament characteristic of preparation is determined by the dynamics that spins thus, the especially region between spinning head outlet and long filament solidification point, and described region is called as cancellation region.The specific design in quenching region, by the airflow rate of the ejaculation long filament of motility still, quenched long filament characteristic is had to very large impact.Conventionally use cross-current to quench and radially quench.After quenching or solidifying, long filament is advanced to roll speed, and the 100-200 of the speed that described speed is normally left from spinneret orifice doubly.Therefore, spin (and stretching) occurs to accelerate at a high speed after spinneret orifice penetrates.The amount of orientation that is frozen into spinning long filament is directly involved in the stress level of solidification point director silk.
The melt-spun filaments making is thus collected in the mode that meets desired final use.For example, 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 canister.Be intended to conventionally be wound on yarn package with conitnuous forms for the long filament of for example distortion, 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, heat setting and untwisting, distortion will be given curling.These multifilament (also referred to as " tow ") comprise with spin-drawing silk (long filament is prepared by it) similar number long filament.Therefore, they preferably comprise at least 10, and at least 25 threads even more preferably, and conventionally can comprise at the most 150 or more, preferably at the most 100, more preferably 80 threads at the most.Yarn has at least 1 conventionally, and more preferably at least 20, preferably at least 50, more preferably at the most 250, and total DENIER of 1,500 at the most.Long filament is preferably at least 0.1dpf, more preferably 0.5dpf at least, more preferably 0.8dpf at least, and 3dpf at the most most preferably.
Can be by PTT/PS-blend melt being spun to long filament at the temperature at 245 to 285 ℃, long filament is quenched, by the filament draw quenching, by the crimped filament stretching, and described long filament is cut into staple fibre, make PTT staple fibre, preferably described staple fibre has the length of 0.2 to 6 inch (0.5 to 15cm).A kind of preferred method comprises: the blend polymer that comprises PTT and 0.1 to 3%PS (a) is provided, (b) at the temperature of 245 to 285 ℃, melt blended material melt spinning is become to long filament, (c) this long filament that quenches, (d) by quenched filament draw, (e) use mechanical crimper, with the long filament of the curling stretching of crimpness of 8 to 30 curling/inch (3 to 12 curling/centimetre), (f) at the temperature of 50 to 120 ℃, make curling long filament lax, and (g) 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, make before curling the long filament stretching anneal at 85 to 115 ℃.Preferably use the roller heating to anneal under tension force.In another preferred embodiment, the long filament of elongation is curling front unannealed.Staple fibre is used yarn and textiles or supatex fabric for the preparation of weaving, and can be used for fibrefill application and manufacture carpet.
Although the present invention mainly describes multifilament, be to be understood that preferred requirement as herein described is to be applicable to monofilament.
Long filament can be circular or have other shape, such as octofoil, triangle, rising sun shape (also referred to as " sol "), scalloped ellipse, trilobal, four flute profiles (also referred to as " four grooves "), scalloped band shape, band shape, radial etc.They can be solid, hollow or porous.
On the other hand, the invention provides the fabric that comprises the long filament that contains composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer in composition, be wherein characterised in that≤3 Denier per filament of long filament ,≤2.5% the DENIER coefficient of variation and at least 0.055 birefringence.In one embodiment, poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
In one embodiment, by endless tow resultant yarn, and fabric is Woven fabric.In 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 fabric.Weave the regular pattern that is characterised in that the interlocking yarn producing by interweave (weaving) or the collar (knitting) with knitted structure.In both cases, yarn meets regular pattern, and they from a side band of fabric to opposite side and return, are gone round and begun again.Formed the integrality of Woven fabric or knitted fabric by fabric self structure.
In supatex fabric, modal, long filament is laid with random patterns, and each other via chemistry or by the use of thermal means rather than mechanical means combination.The example of a commercially available acquisition of the nonwoven producing by these class methods is purchased from DuPont Company spunbond polyester.In some cases, can, by fibrage is laid with complex three-dimensional topology arrays, make nonwoven, described array does not relate to and interweaving or the collar, and wherein fiber does not replace to opposite side, as the United States Patent (USP) 6 people such as Popper from a side wheel, described in 579,815.
Make Woven fabric with many yarns that at right angles interweave each other.The yarn that the yarn that is parallel to fabric length direction is called " warp thread " and orthogonal this direction is called " parallel " or " weft yarn ".Every warp thread is called one " end ".This is found in any fabric or clothes shop, by change interlaced yarns ad hoc fashion, yarn denier, yarn this in aesthetics, yarn density and the warp thread of sense of touch and visual aspects and the ratio of weft yarn, can reach huge change aesthetically.In the ordinary course of things, the structure of Woven fabric gives fabric certain rigidity; The stretching of Woven fabric is generally large less than knitted fabric.
In Woven fabric of the present invention, at least a portion warp thread comprises yarn, it comprises the long filament that contains composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer in composition, be wherein characterised in that≤3 Denier per filament of long filament ,≤2.5% the DENIER coefficient of variation and at least 0.055 birefringence.In one embodiment, poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
In one embodiment, warp thread and weft yarn all comprise yarn, and it comprises long filament herein.In one embodiment, the yarn of long filament and the cotton yarn of at least 40% number herein of containing that warp thread comprises at least 40% number.In one embodiment, the yarn that contains long filament that warp thread comprises at least 80% number, and parallel comprises at least 80% cotton yarn.In the ordinary course of things, the actual demand of warp thread is greater than to weft yarn.
On loom, manufacture Woven fabric, as they modes so always for thousands of years.Although huge change has occurred loom, basic operation logic is identical.Fig. 3 a is the schematic diagram with an embodiment of the loom shown in side view.Place the warp beam 31 being formed by multiple (hundreds of conventionally) parallel end 32 as loom feed.Warp beam 31 is shown in Fig. 3 b with front view.Be shown in Fig. 3 a is biobelt tool loom.Each band tool 34a and 34b are the frameworks that keeps many (hundreds of conventionally) alleged " harness cords ".Referring to Fig. 3 c, the amplification front view with tool 34 is shown, every harness cord 311 is the vertical lines wherein with hole 312.Band tool is set to move up and down, one moves up, and other moves down.Make a part of end 33a pass the hole 312 in the harness cord 311 with tool 34a, and make another part of end 33b through the hole in the lower harness cord with tool 34b, thereby open the gap between end 33a and 33b.In shown type loom, shuttle 36 drives in the mode (being generally wooden paddle) that do not illustrate, with in the time that band tool moves up and down, from a side shifting or shuttle back and forth to opposite side.Shuttle carries weft yarn 37 bobbins, the unwinding in the time that shuttle moves through warp thread tip gap of described bobbin.So-called " reed " or " press strip " the 35th, keep the end framework of freely through a series of vertical lines betwixt.Fig. 3 d is illustrated in the reed 35 of describing vertical line 313 in front view, and the spacing 314 passed through of warp thread.The thickness of vertical line 314 has determined the spacing of the horizontal warp thread of fabric, thereby has determined its density.Reed, for shifting the weft yarn just having inserted onto diagram right side, is arranged and is formed fabric 38.By fabric wrapping on fabric axle 310.Roller 39 is guide rollers.
It is accurate operation that warp beam is reeled, yarn package or the spool of counting similar number with required end are wherein installed conventionally on so-called creel, and each end is delivered in warp beam by a series of accurate guiders and tensioning apparatus, then the disposable coiling of whole warp beam.
The ratio of concrete interlacing pattern, warp thread and weft yarn determines the type of obtained Woven fabric.Basic pattern comprises plain weave, twill-weave and satin weave.Many other more unique weaving-patterns are also known.
Knitting is by one or more yarn is overlapped to the method that makes fabric mutually.Knitted fabric is tending towards having the stretching larger than weaven goods and elasticity.Knitted fabric durability is tending towards lower than weaven goods.In woven situation, there is many knit pattern and knitting type.According to the present invention, fabric is the knit goods that comprises yarn herein in one embodiment, described yarn comprises the long filament that contains composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer in composition, be wherein characterised in that≤3 Denier per filament of long filament ,≤2.5% the DENIER coefficient of variation and at least 0.055 birefringence.In one embodiment, poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
Also imagine in the present invention the clothes by fabric sewing of the present invention.Clothes herein comprises the fabric that contains yarn, described yarn comprises the long filament that contains composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer in composition, be wherein characterised in that≤3 Denier per filament of long filament ,≤2.5% the DENIER coefficient of variation and at least 0.055 birefringence.In one embodiment, poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
Manufacturing clothes by fabric is the technology that non-Changshu is known.Prepare clothes by fabric and comprise and prepare pattern, conventionally prepared by paper wood, or with regard to automatic mode with the preparation of computerization form, measure required pieces of fabric, cutting fabric, to prepare required sheet, is then stitched together described according to described pattern.Clothes can be made one or more patterns of fabric of the present invention specially.Alternatively, clothes can be prepared by the fabric of the present invention and other fabrics that combine one or more patterns.
The present invention is also described in following specific embodiment, but is not subject to their restriction.
example
method of testing
intrinsic viscosity
Use Viscotek Forced kinematic viscosity meter Y900 (Viscorek Corporation, Houston, Tex.) to measure the intrinsic viscosity (IV) of PTT.According to ASTM D-5225-92 method, at 19 ℃, in 50/50 % by weight solvent mixture of trifluoroacetic acid and carrene, form the PTT solution of 0.4g/dl, and measure viscosity.The IV value that these record is associated according to ASTM D4603-96, in phenol/1 of 60/40 % by weight, and the IV value manually recording in 1,2,2-tetrachloroethanes.
number-average molecular weight
Measure the number-average molecular weight of polystyrene according to ASTM D5296-97.Same procedure is for poly-(terephthalic acid (TPA) 1,3-PD ester), and different is that calibration reference is for having 44,000 M wpoly-(Polyethyleneglycol Terephthalate) and hexafluoroisopropanol solvent.
toughness and elongation at break
The physical characteristic of long filament and yarn is used tensile tester 1122 models of Instron Corp. to measure.More specifically, elongation at break E bmeasure according to ASTM D-2256 with toughness.
the impact on result of spinning reciprocating motion and spinning machine
Fibre spinning is carried out in four independent reciprocating motions.As detailed below, reciprocating motion #1,3 and 4 carries out on spinning machine #2, and reciprocating motion #2 carries out on spinning machine #1.
The result obtaining from spinning machine #1 is disperseed, and as shown in table 4 and Fig. 5, and is not considered to reliable.Particularly, the limit that the DENIER coefficient of variation is specified higher than the present invention, and seem not the variation along with the temperature generation systems of the first godet roller.
Fig. 5 is the schematic diagram of DENIER CV to the first seal wire temperature, be wherein obtained from reciprocating motion 1,3 be incorporated in all data of 4 together with and draw diamond curve figure, and the data that derive from reciprocating motion #2 are used triangle mapping.As shown in following table 3-6, not all wherein three the reciprocating data points with spinning machine #2 that are obtained from utilize identical spinning condition to set to obtain.But as shown in Figure 5, the data that derive from spinning machine #2 are shown as rhombus, it shows a clear and definite trend, and wherein the first seal wire temperature is in the scope of about 75 to 85 ℃, corresponding to minimum DENIER CV.In the data of reciprocating motion #2, do not observe similar trend.
To be that short distance DENIER is variational measure the DENIER coefficient of variation, and it is the indication of melt spinning process stability then.Melt spinning process may be unsettled, because spinning component causes unstability.It may be also unsettled, because machine is unsettled.From Fig. 5, be clear that the high DENIER CV producing is in this case the artifact of machine performance and design in reciprocating motion #2.
Spinning machine #1 is the spinning machine that is placed in laboratory, is only provided with the most basic equipment to carry out melt spinning.Conventionally only use spinning machine #1 to obtain the most basic information that whether can be become by melt spinning fiber about experimental group compound.It uses in this paper reciprocating motion #2, and this is because regularly mixing-spinning machine #2 is unavailable on the date of the #2 that regularly moves back and forth.Spinning machine #2 is pilot plant spinning production line.Its condition may extend to full-scale commercial-scale spinning production line completely.This is the spinning production line of selecting the result difference for showing feature of the present invention.
The schematically illustrated spinning machine #2 of Fig. 4.Silo drying machine 41, gravity-fed single screw extrusion machine 42, has dry resin blend pellet.Under pressure, directly feed is in the input of gear pump 43 in the output of single screw extrusion machine 42, and it is provided with overflow port 44.The output of gear pump is supplied to the spin pack 46 of six ends via short (several inches long) transfer line 45, wherein use four ends.Four every velamens that spin in 47 (illustrating one) are extruded (not shown) from 36 hole spinning heads, and wherein each hole characteristic is that diameter is the circular cross section that 0.27mm and length are 0.50mm.Every spins 47 by the cross-current quenching air zone 48 of the about 1.75m of length, wherein surrounding air in reciprocating motion 1 from the effluent spinning to opposite side, and by the radial air quench zone 48 of the about 1.75m of length, wherein surrounding air in reciprocating motion 3 and 4 around the Radial Flow that spins to produce even more uniform long filament.Therefore the contact forming rolls 49 that spins of every quenching, and separate to keep spinning for 6-8 time around the first heating seal wire (feeding roller) 410 and the first corresponding separate roller 411 coiling subsequently.The second separate roller 413 of the second heating seal wire (draw roll) 412 and the second correspondence of leading subsequently that spins, through staggered jet (not shown) and arrive thus wind-up roll 414.Be not shown in addition, the every logical superheated header part of seal wire seals to keep temperature.Extruder is provided with 3 thermals treatment zone and a header area in output.
Spinning machine #1 is substantially the same with spinning machine #2 for the layout described in Fig. 4.Difference is that the quenching ventilation duct in spinning machine #1 is much narrower than its appropriate section on spinning machine #2.
In all examples and comparative example, four average results that spin of spinning simultaneously under every set condition are reported.Before preparation test sample, after changing, setpoint conditions make spinning machine reach stable state by moving about 45 minutes.In the time of the composition change of polymer, clean spinning machine with the PTT containing PS.In the time that spinning head changes, cleaning robot between spinning experiment.
the preparation of blend polymer
By the dry PTT of common feed and PS in the standby PS sample (0.8 and 0.55 % by weight) in PTT of 30mm T/S extrusion mechanism.With the amount shown in table 1, will semi-Dull PTT resin granular material (1.02IV, purchased from DuPont Company (Wilmington, DE)) polytrimethylene-terephthalate and polystyrene (168M KG2, purchased from BASF) pellet mix.Before use that PTT is dry in vacuum drying oven, at 120 ℃, use nitrogen blowing 14 hours.By two kinds of polymer weightless feeding to the 4th cylindrical shell of Wemer & Pfleiderer ZSK-30 reversion double screw extruder respectively.The delivery rate using illustrates with Pounds Per Hour (pph) in table 1.Described extruder has the cylindrical shell that diameter is 30mm, and described cylindrical shell is by forming with two 13 cylindrical shell regions of mediating region and three conveyor zones alternative arrangements, and the L/D ratio that described extruder has is 32.Heat independently in each cylindrical shell region.Region 1-4 is made as 25 ℃, and region 5-13 is made as 210 ℃, 3/16 " strand mould is also made as 210 ℃.Also cylindrical shell region 8 is applied to vacuum.Table 1 also illustrates composition, output speed and the melt temperature of feeding.Extrudate leaves after mould immediately at quenching-in water, then uses standard Granulation Equipments to be a granulated into 1/8 " pellet.
table 1
melt spinning
In four independent spinning reciprocating motions, carry out as mentioned below the melt spinning of fiber.Table 2 is illustrated in and in each reciprocating motion, keeps constant spinning parameter.
reciprocating motion #1-spinning machine #2
So melt compounded pellet dried overnight to moisture in 140 ℃ of dry silos of the PTT/PS blend of preparation is reduced to < 50ppm.In single screw extrusion machine by dry melt blended material gravity feeding in Fig. 4 spinning machine #2 mentioned above.Extruder set point in the 1-3 of region (with ℃) is respectively 230/255/263.By gear pump, extruder is exported to melting feed in spin pack.Spin pack is provided with six spinning sites, and wherein four are provided with spinning head, and each spinning head has 36 holes, and each bore dia is that 0.27mm and length are 0.5mm, and is circular cross section.So every yarn of preparation is 75 DENIER 36 filament yarns.Being arranged on shown in table 3 of the first godet roller.Note the second godet roller to remain on 110 ℃ and 4500rpm.Quenching air is that cross-current quenches, and has the air velocity of 0.35cm/s.
The rules of following are as follows: the second godet roller (draw roll) is set as to 4500m/min and 110 ℃, and does not change at experimental session.Then test with the first godet roller (feeding roller) that is set in 60 ℃, and change speed is to determine the draw ratio that produces high tenacity when adjusting elongation at break to time in the scope of 55-65%.For blend polymer #2 (0.055%PS), find that 2.09 draw ratio causes the highest toughness in the time that elongation at break is in expected range (, feeding roller is set in 2150m/min).Then continue the additional feeding roller temperature spinning with 85 and 110 ℃.Blend polymer #1 (0.8%PS) follows identical operation; Find that 2.37 draw ratio causes the highest toughness in the time that elongation at break is in expected range (, feeding roller speed=1900m/min).
The results are shown in table 3.
Table 3: the result of reciprocating motion #1
reciprocating motion #2-spinning machine #1
In PTT, the novel melting blend of 0.80 % by weight is with above blend #1 is identical.So melt compounded pellet dried overnight to moisture in 140 ℃ of dry silos of the PTT/PS blend of preparation is reduced to < 50ppm.In single screw extrusion machine by dry melt blended material pellet gravity feeding in Fig. 4 spinning machine #1 mentioned above.Extruder set point in the 1-3 of region (with ℃) is respectively 230/255/263.By gear pump, extruder is exported to melting feed in spin pack.Spin pack is provided with six spinning sites, and wherein four are provided with spinning head, and each spinning head has 36 holes, and each bore dia is that 0.27mm and length are 0.5mm, and is circular cross section.So every yarn of preparation is 75 DENIER 36 filament yarns.Being arranged on shown in table 4 of the first godet roller.Note the second godet roller to remain on 110 ℃ and 4500rpm.Quenching air is that cross-current quenches, and has the air velocity of 0.35cm/s.
The rules of following are as follows: the second godet roller (draw roll) is set as to 4500m/min and 110 ℃, and does not change at experimental session.Then test with the first godet roller (feeding roller) that is set in 60 ℃, and change speed is to determine the draw ratio that causes high tenacity when adjusting elongation at break to time in the scope of 55-65%.For blend polymer #1 (0.8%PS), ensuing: to find that 2.37 draw ratio causes the highest toughness in the time that elongation at break is in expected range (, first godet roller speed=1900m/min).
The spinneret hole of example 5 and 6 use diameter 0.27mm is implemented.The spinneret hole of example 7 and 8 use diameter 0.32mm is implemented.Other spinning conditions are shown in table 2 and table 4.The results are shown in table 4.
reciprocating motion #3-spinning machine #2
Use the same crowd of PS/PTT that comprises 0.80 % by weight PS using in reciprocating motion #2.
Use identical spinning machine operation and setting as described in reciprocating motion #1 above to carry out melt spinning, different is in these examples, and spinning 75 DENIER/36 filament yarns and quenching are radially to quench.Spinning condition is shown in table 3 and table 5.Again the extruder thermal treatment zone is set as respectively to 230/255/263 ℃.Spinnerette diameters is 0.27mm.Flow-control is arrived to 37.5g/min.The results are shown in table 5.
reciprocating motion #4--spinning machine #2
With the 3rd blend of method preparation among PTTs the 0.8%PS identical with the method for blend #2 mentioned above.
Use identical spinning machine operation and setting as described in reciprocating motion #3 above to carry out melt spinning, different is spinning 75 DENIER/72 filament yarns in these examples.Spinning condition is shown in table 3 and table 6.Again the extruder thermal treatment zone is set as respectively to 230/255/263 ℃.Spinnerette diameters is 0.27mm.By flow-control, to 37.5g/min, different is to be recorded in here in example 12 and example 13.Result is shown in table 6.

Claims (6)

1. comprise the long filament of composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester) in, the polystyrene of gross weight meter 0.1 to 3 % by weight based on polymer in described composition, wherein said long filament is characterised in that≤3 Denier per filament ,≤2.5% the DENIER coefficient of variation and at least 0.055 birefringence.
2. long filament according to claim 1, wherein said poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
3. long filament according to claim 1, wherein said composition comprises the polystyrene that is dispersed in gross weight meter 0.5 to 2 % by weight in poly-(aromatic dicarboxylic acid 1,3-PD ester), based on polymer in described composition.
4. long filament according to claim 3, the wherein said composition substantially polystyrene of gross weight meter 0.5 to 2 % by weight in poly-by being dispersed in (aromatic dicarboxylic acid 1,3-PD ester), based on polymer in described composition forms.
5. long filament according to claim 2, wherein said composition comprises the polystyrene that is dispersed in gross weight meter 0.5 to 2 % by weight in poly-(terephthalic acid (TPA) 1,3-PD ester), based on polymer in described composition.
6. long filament according to claim 2, the wherein said composition substantially polystyrene of gross weight meter 0.5 to 2 % by weight in poly-by being dispersed in (terephthalic acid (TPA) 1,3-PD ester), based on polymer in described composition forms.
CN201180074821.4A 2011-09-22 2011-09-22 Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom Pending CN103917703A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/US2011/052797 WO2013043180A1 (en) 2011-09-22 2011-09-22 Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom

Publications (1)

Publication Number Publication Date
CN103917703A true CN103917703A (en) 2014-07-09

Family

ID=47914712

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201180074821.4A Pending CN103917703A (en) 2011-09-22 2011-09-22 Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom

Country Status (10)

Country Link
US (1) US20140234623A1 (en)
EP (1) EP2758571A4 (en)
JP (1) JP2014526621A (en)
KR (1) KR20140075743A (en)
CN (1) CN103917703A (en)
BR (1) BR112014006688A2 (en)
CA (1) CA2849238A1 (en)
IN (1) IN2014DN01962A (en)
MX (1) MX2014003498A (en)
WO (1) WO2013043180A1 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2764144A1 (en) * 2011-10-07 2014-08-13 E. I. Du Pont de Nemours and Company Fabric comprising poly(trimethylene arylate) filaments
CN110318277B (en) * 2019-05-10 2020-10-13 上海咏姿时装有限公司 Method for manufacturing burnt-out fabric

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3695025A (en) * 1970-07-30 1972-10-03 Fiber Industries Inc Fibrillated film yarn
CN1662689A (en) * 2002-11-05 2005-08-31 纳幕尔杜邦公司 Poly(trimethylene terephthalate) bicomponent fibers
CN1662357A (en) * 2002-07-11 2005-08-31 纳幕尔杜邦公司 Poly(trimethylene terephthalate) fibers, their manufacture and use
CN101321828A (en) * 2005-12-07 2008-12-10 纳幕尔杜邦公司 Poly(trimethylene terephthalate)/poly(alpha-hydroxy acid) bi-constituent filaments
WO2011022624A1 (en) * 2009-08-20 2011-02-24 E. I. Du Pont De Nemours And Company Poly(trimethylene arylate)/polystyrene composition and process for preparing
WO2011022616A1 (en) * 2009-08-20 2011-02-24 E. I. Du Pont De Nemours And Company Process for producing shaped articles of poly(trimethylene arylate)/polystyrene

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4475330A (en) * 1982-06-03 1984-10-09 Teijin Limited High twist polyester multifilament yarn and fabric made therefrom
US6284370B1 (en) * 1997-11-26 2001-09-04 Asahi Kasei Kabushiki Kaisha Polyester fiber with excellent processability and process for producing the same
JPH11172526A (en) * 1997-11-26 1999-06-29 Asahi Chem Ind Co Ltd Polyester fiber having low thermal stress and spinning thereof
US6923925B2 (en) * 2002-06-27 2005-08-02 E. I. Du Pont De Nemours And Company Process of making poly (trimethylene dicarboxylate) fibers
US7785507B2 (en) * 2004-04-30 2010-08-31 E. I. Du Pont De Nemours And Company Spinning poly(trimethylene terephthalate) yarns

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3695025A (en) * 1970-07-30 1972-10-03 Fiber Industries Inc Fibrillated film yarn
CN1662357A (en) * 2002-07-11 2005-08-31 纳幕尔杜邦公司 Poly(trimethylene terephthalate) fibers, their manufacture and use
CN1662689A (en) * 2002-11-05 2005-08-31 纳幕尔杜邦公司 Poly(trimethylene terephthalate) bicomponent fibers
CN101321828A (en) * 2005-12-07 2008-12-10 纳幕尔杜邦公司 Poly(trimethylene terephthalate)/poly(alpha-hydroxy acid) bi-constituent filaments
WO2011022624A1 (en) * 2009-08-20 2011-02-24 E. I. Du Pont De Nemours And Company Poly(trimethylene arylate)/polystyrene composition and process for preparing
WO2011022616A1 (en) * 2009-08-20 2011-02-24 E. I. Du Pont De Nemours And Company Process for producing shaped articles of poly(trimethylene arylate)/polystyrene

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
TAE HWAN OH等: ""Effect of Polystyrene Mixing on Mechanical Properties and Structural Changes in Melt Spinning"", 《FIBERS AND POLYMERS》 *

Also Published As

Publication number Publication date
CA2849238A1 (en) 2013-03-28
WO2013043180A1 (en) 2013-03-28
US20140234623A1 (en) 2014-08-21
EP2758571A4 (en) 2015-05-20
IN2014DN01962A (en) 2015-05-15
BR112014006688A2 (en) 2017-04-04
KR20140075743A (en) 2014-06-19
EP2758571A1 (en) 2014-07-30
MX2014003498A (en) 2014-07-14
JP2014526621A (en) 2014-10-06

Similar Documents

Publication Publication Date Title
EP3011086B1 (en) Process for the preparation of a fiber, a fiber and a yarn made from such a fiber
CN1662686B (en) Poly(trimethylene dicarboxylate) multifilament and monofilament manufacture method and silk, fabric or carpet prepared therefor
JP3966043B2 (en) Production method of polylactic acid fiber excellent in heat resistance
KR102458368B1 (en) Manufacturing method of self-crimping elastic blended yarn for knitting
CN1662683B (en) Poly(trimethylene terephthalate) bicomponent fiber process
WO2021118985A1 (en) Carpet made from self-bulking ptt-containing bicomponent fibers
US20120009418A1 (en) Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom
CN104105823B (en) Comprise the fabric of poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) long filament
CN103917703A (en) Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom
US8753741B2 (en) Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom
US20180334761A1 (en) Nylon based filaments, yarns, and fabrics
TW202210679A (en) A method to make bicomponent fibers and articles comprising the same
US8540912B2 (en) Process of making poly(trimethylene arylate) fibers
US20110263171A1 (en) Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom
CN111926398B (en) Technological method of super-elastic flame-retardant coarse denier porous PET-DTY
KR102584803B1 (en) High-strength, fine-fine polyester multifilament
WO2017165552A1 (en) Nylon based yarns and fabrics
WO2013055344A1 (en) Process for preparing poly (trimethylene arylate) fibers
WO2002018684A1 (en) Process for making poly (trimethylene terephthalate) yarn

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20140709