CN104105823A - Fabric comprising poly(trimethylene arylate) filaments - Google Patents
Fabric comprising poly(trimethylene arylate) filaments Download PDFInfo
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- CN104105823A CN104105823A CN201180075129.3A CN201180075129A CN104105823A CN 104105823 A CN104105823 A CN 104105823A CN 201180075129 A CN201180075129 A CN 201180075129A CN 104105823 A CN104105823 A CN 104105823A
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- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/50—Woven 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
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- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/20—Woven 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
- D03D15/283—Woven 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
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- 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
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- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D13/00—Woven 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
- D03D13/008—Woven 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
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D10B2321/12—Fibres 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
- D10B2321/121—Fibres 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
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2501/00—Wearing 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
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
Technical field
The present invention relates to method, gained fiber and their purposes for spinning poly (aromatic dicarboxylic acid 1,3-PD ester) fiber.
Background technology
As the fiber that can be used for textiles, form polymer, poly-(aromatic dicarboxylic acid 1,3-PD ester), especially poly-(terephthalic acid (TPA) 1,3-PD ester) (also referred to as 3GT, Triexta or PTT) have been 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 modification polyester yarn prepared by polyethylene terephthalate (PET) and there is widely business application in as spunbond PET in a plurality of textiles purposes as knitting and Woven fabric and supatex fabric.Weaving term " yarn " refers to a branch of filament.For example, shirt and blouse are made by yarn conventionally, and this yarn consists 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 ".Solution 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 a plurality of 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, Fujimoto 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 is compared with PET yarn and to be shown the tensile property of raising, fluffy volume and the feel of improvement.The people such as Howell have described with the spinning speed of 2600m/m at the most and have prepared partially oriented PTT yarn.By contrast, PET carries out melt-spun to be multiple times than the speed of 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 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 for the preparation of spin-drawing.
The PTT spin-drawing filament yarn that needs 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 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, the polystyrene of gross weight meter 0.1 to 3 % by weight ammediol ester), the polymer based 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.
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 described long filament and≤2.5 the DENIER coefficient of variation, described method comprises by having the spinneret orifice extruded polymer fused mass of shape of cross section, it comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester), the polystyrene of gross weight meter 0.1 to 3 % by weight based on described polymer, thereby form continuous thread extrudate, quench this extrudate so that it is solidified into continuous filament yarn, reel on being heated to 70 to 100 ℃ of first driven rollers in temperature range this long filament with the first rotary speed rotation, then reel on being heated to 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, the polystyrene of gross weight meter 0.1 to 3 % by weight ammediol ester), the polymer based 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.
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 charging 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 of using spinning machine #2 to obtain and those results of using 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, the polystyrene of gross weight meter 0.1 to 3 % by weight ammediol ester), the polymer based in described composition, wherein said long filament is characterised in that≤3 Denier per filament (dpf) ,≤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 uses of fabric of thin Denier yarns, such as 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 by having the spinneret orifice extruded polymer fused mass of shape of cross section, it comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, ammediol ester), the polystyrene of gross weight meter 0.1 to 3 % by weight based on described polymer, thereby form continuous thread extrudate, quench this extrudate so that it is solidified into continuous filament yarn, reel on being heated to 70 to 100 ℃ of first driven rollers in temperature range this long filament with the first rotary speed rotation, then reel on being heated to 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 when 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 Yarn 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 the value by obtaining divided by average DENIER with DENIER standard deviation, with Uster tester, measures.
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 are expressed as the polystyrene percentage by weight with respect to the total polymer weight in composition.
Unless stated otherwise, when providing number range herein, should understand the end points of its covering scope.Should understand, the precision of the number of significant figures providing as described in ASTM E29-08 is provided numerical value.For example, numeral 3 should be understood the scope that contains 2.5 to 3.4, and numeral 3.0 should be understood the scope that contains 2.95 to 3.04.
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 difference of the special acrylate monomers unit molecular weight that when the present invention extends to other poly-(aromatic dicarboxylic acid 1,3-PD esters), reply concentration adjustment is by weight suitable for relating to.
The homopolymers of polystyrene and PTT and copolymer are all applicable to the present invention.For purposes of the present invention, term " copolymer " should be understood and not only contains 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 PS of the PTT that described composition comprises 70 to 99.5 % by weight, 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 comprised of composition substantially, and described composition is comprised 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 comprised of composition substantially, described composition substantially by the PTT of 70 to 99.5 % by weight, the PS of 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 comprised of composition substantially, and described composition is comprised 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; (except 1,3-PD) straight chain, ring-type and the side chain aliphatic diol with 2-8 carbon atom, for example ethylene glycol, 1,2-PD, 1,4-butanediol, 3-methyl isophthalic acid, 5-pentanediol, 2,2-dimethyl-1, ammediol, 2-methyl isophthalic acid, ammediol and Isosorbide-5-Nitrae-cyclohexanediol; And aliphatic series and the aromatic oxide glycol with 4-10 carbon atom, for example two (2-ethoxy) ether of hydroquinones or have poly-(ether) 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 the content of 30 % by mole exists at the most.
Described PTT can comprise other selected comonomers of trace so that they 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 polyblends 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) in 0.70dl/g to 2.0dl/g scope.In another embodiment, suitable PTT is characterised in that the IV in 0.80dl/g to 1.5dl/g scope.In another embodiment, suitable PTT is characterised in that the IV in 0.90dl/g to 1.2dl/g scope.
In one embodiment, suitable PTT is characterised in that 20,000Da to 25, 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 M within the scope of 000Da
n.In another embodiment, the M of polystyrene homopolymer
n50,000Da to 200, in the scope of 000Da.In another embodiment, the M of polystyrene homopolymer
n75,000Da to 200, in the scope of 000Da.In another embodiment, the M of polystyrene homopolymer
n120,000Da to 150, in 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, comprises Dow Chemical Co. (Midland, Mich.), BASF (Mount Olive, N.J.) and Sigma-Aldrich (Saint Louis, Mo.).
By PTT and PS melt blending, then with strand form, extrude, be cut into subsequently pellet.Also can carry out other forms of melt blending and pulverizing subsequently, as formed 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 fused mass to form the second melt blended material with additional PTT again 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.Yet blend will have other compositions in many cases, such as being generally comprised within polyester polymer composition for 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 seven property.Add therein in those situations of polymer additional, non-polyester, polyester keeps identical with those compositions that do not comprise other polymer with the ratio of the weight percent concentration of PS.
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 monomer 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 the melt blended material that (a) preparation is comprised of PTT and 0.1 to 3 % by weight (wt%) polystyrene (PS) substantially, and the polymer melting blend that (b) solution 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 in spin-drawing method, to put on the direct result of the high tensile force of long filament.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 solution 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 via weightless charger 4 or other pellet feeding manner chargings in 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 swim from it charging in double screw extruder 3.In double screw extruder, form PTT/PS melt blended material.Gained melt blended material in the spinning block that comprises spinning head 8, is extruded one or more continuous filament yarn 9 by described spinning head via transfer line 7 chargings.
Fig. 2 has described according to the present invention for a kind of suitable structure of solution spinning.34 threads 22 (all 34 threads are not shown) are extruded by hole spinning head 21.Long filament forms 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 flows radially outward 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 feed roller) and the separate roller of 70 to 100 ℃.Yarn is reeled 6 to 8 times on the first godet roller and separate roller.Yarn is from the first godet roller by being made as the second driving godet roller (being also called draw roll) of 110 to 130 ℃, and described second drives godet roller to connect with the second separate roller.Yarn is reeled 6 to 8 times on the second godet roller and separate roller.Draw roll speed is 4000 to 6000m/min, and the ratio of draw roll speed and feed 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 on the 3rd pair roller.Yarn by staggered jet 28, then leads to mate the wind-up roll 29 of the speed running of 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 this part long filament 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 this 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 controlled wind-up roll of tension force.
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 falls 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.The long filament that merging is so extruded is to form yarn.Conventionally by applying some, stir, twisting or both are 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 merges to prepare the long filament number of yarn unrestricted.
Yarn formed according to the present invention is not limited only to consist 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 yarn that form, formed according to the present invention is applicable by spin-drawing method mentioned above make false twist texturized charging 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 above-mentioned spinning technique; (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 in the downstream of rotary spindle, make upstream twisting untwisting, 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 spinning.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 comprised of long filament of the present invention can be used for multiple uses of fabric, only need in the textile 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≤200nm of PS particle in PTT matrix.
Favorable characteristics of the present invention comprises can be with the ability of 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 applying of melt blending of enough high shears then.There is not spinning properties and/or the unexpected threshold value granularity declining of physical characteristic at 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, for the distribution of particles in PTT matrix, there is not specific uniformity threshold value.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 uses of fabric.Unless the method that PS is dispersed in PTT is characterised in 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 depend on the rotating speed of hybrid element, the viscosity of fused mass and fused mass in time of staying of 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 so-called high-shear mixer field as mixing in 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 rear feeding in spinning machine, or can be by the direct charging of melt blended material 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 from the charging of satellite extruder in the Mixed Zone of double screw extruder, thereby form melt blended material.In another approach, in charging, before double screw extruder carries out melt blending, can be dry mixed by rolling the polymer of not melting.
From good fibre spinning performance perspective, the particle mean size that is greater than 500nm is not preferred.In addition, the even continuous yarn spinning along single end mode and end to end system obviously all depends on 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 to spinning head via transfer line.Fused mass by extruder input transfer line is disorderly.Yet spinning head charging is necessary for laminar flow, during with a plurality of 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 so mechanical performance of the fiber of generation 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 130 ℃ and <-40 ℃.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 charging in 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 controlled-volume the spin pack of heating via transfer line.Pump must provide the pressure of 10-20MPa to force fluid to pass through spin pack, and described spin pack comprises filter medium (for example casting bed and sieves), to remove any particle that is greater than several microns.By measuring pump, controlled by the mass flowrate of spinning head.In sub-assembly bottom, polymer leaves and enters gas quenching region via a plurality of apertures in metal thick plate (spinning head).Although hole number 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 ℃, realize spinning.
Exemplary traffic by this size hole is tending towards in the scope of 1-5g/min.Adopt multiple spinneret orifice shape of cross section, yet circular cross section is modal.Conventionally, by its screw spin the rotating roller system control line speed of high degree of controlled of long filament.Filament diameter is by flow and batch speed and determine; And can't help spinneret orifice size, determine.
The long filament characteristic of preparation is determined by the dynamics that spins thus, the region between spinning head outlet and long filament solidification point especially, and described region is called as quenching region.The specific design in quenching region, the airflow rate by the ejaculation long filament of motility still have very large impact to the long filament characteristic of quenching.Conventionally use cross-current quench and radially quench both.After quenching or solidifying, long filament is advanced to batch 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 levels of solidification point director silk.
The melt-spun filaments making is thus collected to meet the mode of 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 for the long filament such as distortion, conventionally be wound on yarn package with conitnuous forms, 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 nearly 150 or more, preferably nearly 100,80 threads nearly more preferably.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, 0.5dpf at least more preferably, 0.8dpf at least more preferably, and 3dpf at the most most preferably.
Can be by PTT/PS-blend solution 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 solution is spun to long filament, (c) this long filament that quenches, (d) by the filament draw quenching, (e) use mechanical crimper, long filament with 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 stretching 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 shapes, 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, the polystyrene of gross weight meter 0.1 to 3 % by weight ammediol ester), the polymer based 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.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 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 fabric.Weave with knitted structure and be characterised in that the interlocking yarn regular pattern making by interweave (weaving) or the collar (knitting).In both cases, the yarn pattern that follows the principles, from a side band of fabric to opposite side and return, goes round and begins again them.By fabric self structure, form and weave or the integrality of knitted fabric.
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.
With many yarns that at right angles interweave each other, make Woven fabric.The yarn that the yarn that is parallel to fabric length direction is called " warp thread " and this direction of quadrature is called " parallel " or " weft yarn ".Each 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.As universal law, the structure of Woven fabric is given certain rigidity to fabric; 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, the polystyrene of gross weight meter 0.1 to 3 % by weight ammediol ester), the polymer based 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.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 described yarn comprises long filament herein.In one embodiment, the yarn of long filament and the cotton yarn of at least 40% number herein of comprising that warp thread comprises at least 40% number.In one embodiment, the yarn that comprises long filament that warp thread comprises at least 80% number, and weft yarn 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 the embodiment of loom shown in side view.The warp beam 31 that placement is comprised of a plurality of (hundreds of conventionally) parallel end 32 is as loom charging.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 move down.A part of end 33a is passed with the hole 312 in the harness cord 311 of tool 34a, and make another part of end 33b through lower to the hole in the harness cord of 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 when 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 when 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 is 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 than the larger stretching of weaven goods and elasticity.Knitted fabric durability is tending towards lower than weaven goods.With regard to weaving, there is many knit pattern and knitting style.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, the polystyrene of gross weight meter 0.1 to 3 % by weight ammediol ester), the polymer based 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.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, the polystyrene of gross weight meter 0.1 to 3 % by weight ammediol ester), the polymer based 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.In one embodiment, poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
By fabric, manufacturing clothes is the technology that non-Changshu is known.By fabric knitting clothes, comprise preparation pattern, conventionally by paper wood, prepare, or with form of computers, prepare with regard to automation process, 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 combining fabric of the present invention and other fabrics of 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 flow viscosimeter Y900 (Viscorek Corporation, Houston, Tex.) to measure the intrinsic viscosity (IV) of PTT.According to ASTM D-5225-92 method, at 19 ℃, in the solvent mixture of 50/50 % by weight 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
According to ASTM D5296-97, measure the number-average molecular weight of polystyrene.Same procedure is for poly-(terephthalic acid (TPA) 1,3-PD ester), and different is that calibration standard 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 types of Instron Corp. to measure.More specifically, elongation at break Eb and toughness are measured according to ASTM D-2256.
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 DENIER coefficient of variation is higher than the limit of appointment of the present invention, and seems 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 together with all data of 4 are incorporated in and draw diamond curve figure, and the data that derive from reciprocating motion #2 is used triangle mapping.As shown in following table 3-6, not all being obtained from wherein utilizes identical spinning condition to set to obtain by three reciprocating data points of spinning machine #2.Yet 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 solution spinning.Whether conventionally only use spinning machine #1 to obtain can be by the most basic information of solution spinned 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 to select for showing the spinning production line of the result difference of feature of the present invention.
The schematically illustrated spinning machine #2 of Fig. 4.Silo drying machine 41, the single screw extrusion machine 42 of gravity charging, has dry resin blend pellet.Under pressure, directly charging is in the input of gear pump 43 in the output of single screw extrusion machine 42, and gear pump 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 is characterised in 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 radially quenching air 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 spinning of every quenching contacts forming rolls 49, and around the first heating seal wire (feed roller) 410 and the first corresponding separate roller 411 coiling, spins separately for 6-8 time with maintenance 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 of seal wire partly seals to keep temperature.Extruder is provided with 3 thermals treatment zone and a Head Section 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 have been reported.Before preparation test sample, after changing, setpoint conditions make spinning machine reach stable state by moving about 45 minutes.When the composition change of polymer, with the PTT containing PS, clean spinning machine.When spinning head changes, cleaning robot between spinning experiment.
the preparation of blend polymer
By co-fed dry PTT 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)) poly-(terephthalic acid (TPA) 1,3-PD ester) mixes with polystyrene (168M KG2, purchased from BASF) pellet.Before use that PTT is dry in vacuum drying oven, at 120 ℃, use nitrogen blowing 14 hours.Two kinds of polymer are distinguished to weightless charging in the 4th cylindrical shell region of Werner & Pfleiderer ZSK-30 reversion double screw extruder.The feed rate of 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 section 8 is applied to vacuum.Table 1 also illustrates composition, output speed and the melt temperature of charging.Extrudate leaves after mould immediately at quenching-in water, then uses standard Granulation Equipments to be a granulated into 1/8 " pellet.
table 1
solution spinning
In four independent spinning reciprocating motions, carry out as mentioned below the solution 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 charging in Fig. 4 spinning machine #2 mentioned above.Extruder set point in the 1-3 of region (℃) be respectively 230/255/263.By gear pump, extruder is exported to melting charging 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.Attention remains on 110 ℃ and 4500rpm by the second godet roller.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 with the first godet roller (feed roller) that is set in 60 ℃, test, 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 when elongation at break is in expected range (, feed roller is set in 2150m/min), 2.09 draw ratio causes the highest toughness.Then continue the other feed roller temperature spinning with 85 and 110 ℃.Blend polymer #1 (0.8%PS) follows identical rules; Find when elongation at break is in expected range (, feed roller speed=1900m/min), 2.37 draw ratio causes the highest toughness.
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 charging in Fig. 4 spinning machine #1 mentioned above.Extruder set point in the 1-3 of region (℃) be respectively 230/255/263.By gear pump, extruder is exported to melting charging 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.Attention remains on 110 ℃ and 4500rpm by the second godet roller.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 with the first godet roller (feed roller) that is set in 60 ℃, test, 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: find when elongation at break is in expected range (, first godet roller speed=1900m/min), 2.37 draw ratio causes the highest toughness.
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
The same crowd of PS/PTT that comprises 0.80 % by weight PS that use is used in reciprocating motion #2.
Solution spinning is carried out in identical spinning machine method and the setting of use as described in reciprocating motion #1 above, and 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
The 3rd blend with the identical method preparation 0.8%PS in PTT of the method with blend #2 mentioned above.
Solution spinning is carried out in identical spinning machine method and the setting of use as described in reciprocating motion #3 above,
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 (8)
1. the fabric that comprises long filament, described long filament comprises composition, described composition comprises and is dispersed in poly-(aromatic dicarboxylic acid 1, the polystyrene of total polymer weight meter 0.1 to 3 % by weight ammediol ester), based in described composition, wherein said long filament is characterised in that≤3 Denier per filament ,≤3% the DENIER coefficient of variation and at least 0.055 birefringence.
2. fabric according to claim 1, wherein said poly-(aromatic dicarboxylic acid 1,3-PD ester) is poly-(terephthalic acid (TPA) 1,3-PD ester).
3. fabric according to claim 1, wherein said composition comprises and is dispersed in polystyrene in poly-(aromatic dicarboxylic acid 1,3-PD ester), total polymer weight meter 0.5 to 2 % by weight based in described composition.
4. fabric according to claim 3, wherein said composition substantially polystyrene in poly-by being dispersed in (aromatic dicarboxylic acid 1,3-PD ester), total polymer weight meter 0.5 to 2 % by weight based in described composition forms.
5. fabric according to claim 2, wherein said composition comprises and is dispersed in polystyrene in poly-(terephthalic acid (TPA) 1,3-PD ester), total polymer weight meter 0.5 to 2 % by weight based in described composition.
6. fabric according to claim 2, wherein said composition substantially polystyrene in poly-by being dispersed in (terephthalic acid (TPA) 1,3-PD ester), total polymer weight meter 0.5 to 2 % by weight based in described composition forms.
7. fabric according to claim 1, wherein said fabric is Woven fabric.
8. clothes, comprises fabric claimed in claim 1.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/US2011/055404 WO2013052065A1 (en) | 2011-10-07 | 2011-10-07 | Fabric comprising poly(trimethylene arylate) filaments |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104105823A true CN104105823A (en) | 2014-10-15 |
| CN104105823B CN104105823B (en) | 2016-06-15 |
Family
ID=44872610
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201180075129.3A Expired - Fee Related CN104105823B (en) | 2011-10-07 | 2011-10-07 | Comprise the fabric of poly-(aromatic dicarboxylic acid 1,3-propylene glycol ester) long filament |
Country Status (8)
| Country | Link |
|---|---|
| EP (1) | EP2764144A1 (en) |
| JP (1) | JP5964437B2 (en) |
| KR (2) | KR20140074984A (en) |
| CN (1) | CN104105823B (en) |
| BR (1) | BR112014007745A2 (en) |
| CA (1) | CA2850492A1 (en) |
| MX (1) | MX2014004059A (en) |
| WO (1) | WO2013052065A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111788342A (en) * | 2018-03-02 | 2020-10-16 | 东丽株式会社 | Twisted cord made of liquid crystal polyester multifilament, process for producing the same, and product obtained by using the same |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101646338B1 (en) * | 2014-08-20 | 2016-08-16 | 도레이첨단소재 주식회사 | Polyester nonwoven fabric having an improved softness and mechanical property and manufacturing method thereof |
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| US5993712A (en) * | 1997-02-25 | 1999-11-30 | Lurgi Zimmer Aktiengesellschaft | Process for the processing of polymer mixtures into filaments |
| JP2001151997A (en) * | 1999-11-30 | 2001-06-05 | Toray Ind Inc | Melt spinning polyester composition, polyester high orientation undrawn yarn and its production method |
| CN1662686A (en) * | 2002-06-27 | 2005-08-31 | 纳幕尔杜邦公司 | Poly(trimethylene dicarboxylate) fibers, their manufacture and use |
| 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 |
| 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 |
Family Cites Families (9)
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| US6107220A (en) | 1996-10-18 | 2000-08-22 | E. I. Du Pont De Nemours And Company | Rapid fabric forming |
| US6284370B1 (en) | 1997-11-26 | 2001-09-04 | Asahi Kasei Kabushiki Kaisha | Polyester fiber with excellent processability and process for producing the same |
| JPH11189925A (en) * | 1997-12-22 | 1999-07-13 | Toray Ind Inc | Production of sheath-code conjugated fiber |
| US6287688B1 (en) | 2000-03-03 | 2001-09-11 | E. I. Du Pont De Nemours And Company | Partially oriented poly(trimethylene terephthalate) yarn |
| GB2371567A (en) * | 2001-01-26 | 2002-07-31 | Du Pont | Calendered fabric for ultraviolet light protection |
| JP3862996B2 (en) * | 2001-10-31 | 2006-12-27 | 帝人ファイバー株式会社 | Polytrimethylene terephthalate filament yarn and method for producing the same |
| JP4073238B2 (en) * | 2002-04-19 | 2008-04-09 | 旭化成せんい株式会社 | Clothing |
| US7785507B2 (en) | 2004-04-30 | 2010-08-31 | E. I. Du Pont De Nemours And Company | Spinning poly(trimethylene terephthalate) yarns |
| EP2758571A4 (en) * | 2011-09-22 | 2015-05-20 | Du Pont | Poly(trimethylene arylate) fibers, process for preparing, and fabric prepared therefrom |
-
2011
- 2011-10-07 WO PCT/US2011/055404 patent/WO2013052065A1/en active Application Filing
- 2011-10-07 KR KR1020147012064A patent/KR20140074984A/en not_active Application Discontinuation
- 2011-10-07 BR BR112014007745A patent/BR112014007745A2/en not_active Application Discontinuation
- 2011-10-07 EP EP11773940.9A patent/EP2764144A1/en not_active Withdrawn
- 2011-10-07 CN CN201180075129.3A patent/CN104105823B/en not_active Expired - Fee Related
- 2011-10-07 MX MX2014004059A patent/MX2014004059A/en not_active Application Discontinuation
- 2011-10-07 CA CA2850492A patent/CA2850492A1/en not_active Abandoned
- 2011-10-07 JP JP2014534525A patent/JP5964437B2/en not_active Expired - Fee Related
- 2011-10-07 KR KR1020187003715A patent/KR101952553B1/en active IP Right Grant
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|---|---|---|---|---|
| US5993712A (en) * | 1997-02-25 | 1999-11-30 | Lurgi Zimmer Aktiengesellschaft | Process for the processing of polymer mixtures into filaments |
| JP2001151997A (en) * | 1999-11-30 | 2001-06-05 | Toray Ind Inc | Melt spinning polyester composition, polyester high orientation undrawn yarn and its production method |
| CN1662686A (en) * | 2002-06-27 | 2005-08-31 | 纳幕尔杜邦公司 | Poly(trimethylene dicarboxylate) fibers, their manufacture and use |
| 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 |
| 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 |
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| HOE H.CHUAH: "Intrinsic Birefringence of Poly(trimethylene terephthalate)", 《JOURNAL OF POLYMER SCIENCE PART B :POLYMER PHYSICS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111788342A (en) * | 2018-03-02 | 2020-10-16 | 东丽株式会社 | Twisted cord made of liquid crystal polyester multifilament, process for producing the same, and product obtained by using the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP5964437B2 (en) | 2016-08-03 |
| CN104105823B (en) | 2016-06-15 |
| KR101952553B1 (en) | 2019-02-26 |
| KR20180019750A (en) | 2018-02-26 |
| WO2013052065A1 (en) | 2013-04-11 |
| JP2014528521A (en) | 2014-10-27 |
| EP2764144A1 (en) | 2014-08-13 |
| BR112014007745A2 (en) | 2017-04-11 |
| KR20140074984A (en) | 2014-06-18 |
| CA2850492A1 (en) | 2013-04-11 |
| MX2014004059A (en) | 2014-06-05 |
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