CN1210449C - Method for spinning and winding of polyester filaments using spinning additives, polyester filaments obtained by spinning method, draw texturing of polyester filaments and bulked polyester filaments - Google Patents
Method for spinning and winding of polyester filaments using spinning additives, polyester filaments obtained by spinning method, draw texturing of polyester filaments and bulked polyester filaments Download PDFInfo
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- CN1210449C CN1210449C CNB018102972A CN01810297A CN1210449C CN 1210449 C CN1210449 C CN 1210449C CN B018102972 A CNB018102972 A CN B018102972A CN 01810297 A CN01810297 A CN 01810297A CN 1210449 C CN1210449 C CN 1210449C
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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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to a method for the production and winding of pre-oriented polyester filaments, comprising at least 90 wt. %, based on the total weight of polyester filament, polybutylene terephthalate (PBT) and/or polytrimethylene terephthalate (PTMT), preferably PTMT, characterised in that a) the spinning draft is set in the range 70 to 500, b) directly after exiting the spinning nozzle, the filaments run through a cooling delay zone of 30 mm to 200 mm in length, c) the filaments are cooled to below the solidification temperature, d) the filaments are bundled at a separation of between 500 mm and 2500 mm from the bottom face of the nozzle, e) the thread tension, before and between the drawing galettes is set to between 0.05 cN/dtex and 0.20 cN/dtex, f) the threads are wound with a thread tension of between 0.025 cN/dtex and 0.15 cN/dtex, g) the winding speed is set to between 2200 m/min and 3500 m/min and h) a polyester is used with 0.05 wt. % to 2.5 wt. %, based on the total weight of the filament, of added additive polymer as extensibility improver.
Description
The present invention relates to a kind of by using the spinning additive spinning and reel based on the polyester filament gross weight, be not less than polybutylene terephthalate (PBT) (PBT) and/or the polytrimethylene-terephthalate (PTMT) of 90wt%, the method for the POY polyester filament of preferred PTMT and also relate to can be by the POY polyester filament of this method acquisition.The present invention relates to further also that stretcher strain is spun into and the method for the polyester filament of reeling and also relate to the varicosity polyester filament that can therefore obtain.
The production of continuous polyester filament and particularly polyethylene terephthalate (PET) is known in two step method.In the method, first step comprises spinning and the flat POY long filament of reeling, with this POY long filament in second step fully stretching become bulk filament with heat setting or stretcher strain.
The general introduction in this field is provided by the books Synthetishe Fasern of F.Fourn é, and these books are by Hanser, and publish in Munich.Yet, only describe the production of PET fiber and do not provide unified spining technology, the description general introduction of different features is only arranged.
But from various spinning polymers, comprise polypropylene, polyamide, the fiber production of polyester etc., the part of formation DE-A 38 19 913 purposes.Yet, the production of PET fiber has only been described in an embodiment, as can discerning from the temperature of processable polymer.
About the problem of producing continuous polytrimethylene-terephthalate (PTMT) or polybutylene terephthalate (PBT) (PBT) long filament is the POY long filament, not only directly after spinning and in coiling also after reeling several hours, in the storage process at room temperature, show the suitable tendency of shrinking, it causes yarn to shorten.Be to make that the package meeting is shunk solid on winding mandrels and can not be removed again under special situation with the package compression result.In addition, the package meeting produces the so-called saddleback with hard edge and waist shape core.The result is, the textiles data of long filament as this paricular value of crow, become more inhomogeneous and go wrong when the package debatching.Such problem does not occur in the processing of PET fiber.
Further observe, with the difference of PET long filament contrast, POY PBT or PTMT long filament are aging very fast in storage process.Structure hardening takes place and causes that boiling water shrinks the degree that reduces to bigger and makes and can detect post crystallization.Such PBT or PTMT long filament only part are applicable to that further processing is that they cause the defective in the stretcher strain and cause the remarkable reduction of textured yarns fracture strength.
On the one hand for PET be attributable to structure and performance difference for the difference between PBT and the PTMT on the other hand, for example at Chemical Fibers Int., 53 pages, that reports in 50 volumes (2000) and discuss in the 39th the international artificial fibre conference of 13-15 day in September of Dornbirn is such.Therefore believe that it is the reason of performance difference that different chains forms.
The first string that is used to address these problems is described in WO99/27168 and EP0, and 731, among the 196B1.WO99/27168 has described a kind of polyester fiber, and it is 90wt% polytrimethylene-terephthalate and boiling water is punctured into 5%-16% and extension at break is 20%-60% at least.The polyester fiber of describing in WO99/27168 is produced by spinning and stretching.The maximum spinning withdrawal speed of report is 2100m/min.Because low spinning speed the method is uneconomic.In addition, the polyester fiber of acquisition, as the Parameter File of report, be highly crystalline and therefore only part be applicable to the stretcher strain method.
EP 0,731, and 196B1 has described by after stretching and before reeling yarn being heat-treated the method for spinning, stretching and coiling synthetic threads with the tendency that reduces its contraction.Operable synthetic fiber comprise the polytrimethylene-terephthalate fiber.At EP0,731, among the 196B1, by with synthetic threads closely near but substantially contactlessly heat-treat along prolonging area of heating surface guiding.Heat treated apply increased the technology cost and, in addition, provide synthetic threads with high-crystallinity, it only part be applicable to pull-shaped deformation method.
The article of Dr.H.S.Brown and H.H.Chuah " based on the distortion of polytrimethylene-terephthalate's textiles filament yarn ", Chemical Fibers International, 47 volumes, in February, 1997, the 72-74 page or leaf has been described the stretcher strain of POY polytrimethylene-terephthalate long filament under 450m/min and 850m/min deformation velocity.According to this disclosure, owing to obtain to have the fiber of better material property in the case, the lower deformation velocity of 450m/min is more suitable for polytrimethylene-terephthalate's long filament.It is 38.0% (deformation velocity 450m/min) and 33.5% (deformation velocity 850m/min) that polytrimethylene-terephthalate fiber's fracture strength is reported to 26.5cN/tex (deformation velocity 450m/min) and 29.15cN/tex (deformation velocity 850m/min) and extension at break.
WO 01/04393 has described the PTMT long filament that boiling water is punctured into 3-40%.Yet, after forming long filament, measure this numerical value immediately.This numerical value is reduced to less than 20% in storage 4 all processes under standard conditions, as by accompanying drawing 1 proof.
Fig. 1 has described for the boiling water contraction change of three kinds of PTMT POY bobbins as period of storage function under standard conditions.Three bobbins of research have different initial values.Bobbin #16 and 17 has＞40% high initial value, the boiling water after 4 weeks shrink greater than 30% be preferably greater than 40%.Yet, when initial boiling water shrinkage value less than 40% the time, the boiling water shrinkage value can be reduced to below 30% the critical value after storing in 4 weeks clearly from bobbin 18.
It is measuring of fiber process performance and degree of crystallinity that boiling water shrinks.The fiber of describing in WO 01/04393 comprises the plastics with comparable high-crystallinity, and they significantly more are difficult to processing and only can process at lower draw ratio and/or under lower deformation velocity.
The purpose of this invention is to provide a kind of production and reel, be not less than the method for the POY polyester filament of the PBT of 90wt% and/or PTMT, the POY polyester filament of therefore producing simply and reel based on the long filament gross weight.More particularly, the extension at break numerical value of POY polyester filament should be 90%-165%, about the high uniformity and the same low-crystallinity of long filament parameter.
Further purpose of the present invention provides the economic commercial run of spinning and coiling POY polyester filament.Method of the present invention should allow very high spinning withdrawal speed, is preferably greater than 2200m/min and greater than the high yarn weight of 4kg in package.
Of the present invention still further purpose be to improve the storage of the POY polyester filament that can obtain by the inventive method.They should store the time of prolongation, for example 4 weeks.Ideally, package should not densification in storage process, particularly is not taken in to shrink solid on the winding mandrels and form the saddleback with hard edge and waist shape core, and is no problem when making from package unwinding.
According to the present invention, the POY polyester filament should particularly under high deformation velocity, be preferably greater than 450m/min simply with further processing in stretching or stretcher strain operation.Can should have excellent material property by the long filament that stretcher strain obtains, for example greater than the high fracture strength of 26cN/tex and for the HE long filament greater than 30% high extension at break and for the SET long filament greater than 36% high extension at break.
Therefore the invention provides a kind of production and coiling gross weight based on polyester filament, be not less than polybutylene terephthalate (PBT) (PBT) and/or the polytrimethylene-terephthalate (PTMT) of 90wt%, the method of the POY polyester filament of preferred PTMT is characterized in that this method comprises:
A) spin the journey draw ratio in the setting of 70-500 scope,
B) will be directly from the long filament in spinning head exit length by quenching delay zone 30mm-200mm,
C) long filament is quenched to below the solidification temperature,
D) long filament is restrained in the distance from spinning head bottom surfaces (underface) 500mm-2500mm,
E) be set in the unwinding godet roller above and between yarn tension be 0.05cN/dtex-0.20cN/dtex,
F) under the yarn tension of 0.025cN/dtex-0.15cN/dtex, batch yarn,
G) setting coiling speed is 2200m/min-6000m/min,
H) and in mixture, use and comprise based on the polyester of long filament gross weight as the additive polymer extensibility reinforcing agent of 0.05wt%-2.5wt%.
This unpredictalbe method provides POY polyester filament, it in addition under standard conditions, store the elite clone performance that keeps them after 4 weeks.Do not observe because the contraction of the fiber that is spun on the remarkable deterioration of aging yarn evenness numerical value and the bobbin.
Simultaneously, method of the present invention has many further advantages.These comprise:
Method of the present invention simple and economical on big commercial scale, to implement.More particularly, this method allows spinning under the high withdrawal speed of 2200m/min at least and coiling and the maintenance production greater than the package of the high yarn weight of 4kg.
The use of spinning additive makes can reach the withdrawal speed of 6000m/min at the most.The result is an operating equipment especially economically.
Therefore can stretch or the stretcher strain operation in, simply, economically and on big commercial scale the further processing POY polyester filament that can obtain by this method.In operation, can under speed, be out of shape greater than 450m/min.
Because the high evenness of the POY polyester filament that can obtain by this method, reach good package simply to guarantee the further processing of all even flawless substantially dyeing and POY polyester filament.
Can have by the long filament that stretcher strain obtains greater than the high fracture strength of 26cN/tex and for the HE long filament greater than 30% high extension at break and for the SET long filament greater than 36% high extension at break.
The invention provides and produce and reel, be not less than the method for the polybutylene terephthalate (PBT) (PBT) of 90wt% and/or polytrimethylene-terephthalate's (PTMT) POY polyester filament based on the long filament gross weight.Polybutylene terephthalate (PBT) (PBT) and/or polytrimethylene-terephthalate (PTMT) are known for those skilled in the art.Polybutylene terephthalate (PBT) (PBT) can be by terephthalic acid (TPA) and equimolar amounts 1, and the polycondensation acquisition of 4-butanediol and polytrimethylene-terephthalate can be by terephthalic acid (TPA) and equimolar amountss 1, and the polycondensation of ammediol obtains.The mixture of two kinds of polyester also is conceivable.According to the present invention, PTMT preferably.
Polyester can be homopolymers or copolymer.Useful copolymer is particularly including such copolymer, this copolymer, and PTMT and/or PBT repetitive, comprise the repetitive of the following common monomer of 15mol% (based on all repetitives of polyester) at the most: for example ethylene glycol, diethylene glycol (DEG), triethylene glycol, 1,4 cyclohexane dimethanol, polyethylene glycol, M-phthalic acid and/or adipic acid.Yet, for purpose of the present invention, preferably polyester homopolymer.
Polyester of the present invention can comprise the other additive as mixture of common amount, absorbs improver, light stabilizer, organic phosphite, fluorescent whitening agent and delustering agent as catalyst, stabilizing agent, antistatic additive, antioxidant, fire retardant, dyestuff, dyestuff.Preferably, polyester comprises the 0-5wt% additive, based on the gross weight of long filament.
Polyester can further comprise small part, and the preferred branching agent of 0.5wt% (brancher) component at the most is based on the long filament gross weight.Preferred branched agent component according to the present invention comprises the polyfunctional acid, and as trimellitic acid, or pyromellitic acid, or three to sexavalence alcohol, as trimethylolpropane, pentaerythrite, dipentaerythritol, glycerine or corresponding carboxylic acid.
In the context of the present invention, PBT and/or PTMT are mixed with the additive polymer as the extensibility reinforcing agent based on long filament gross weight 0.05wt%-2.5wt%.The useful especially additive polymer that is used for the object of the invention comprises the polymer and/or the copolymer of following provisions:
1. the copolymer that comprises following monomeric unit:
A=acrylic acid, methacrylic acid or CH
2=CR-COOR ', wherein R is H atom or CH
3Group and R ' are C
1-15Alkyl or C
5-12Cycloalkyl or C
6-14Aryl,
B=styrene or C
1-3The styrene that alkyl replaces,
Copolymer is by the A of 60-98wt% and the B of 2-40wt%, the A of preferred 83-98wt% and the B of 2-17wt% and more preferably the B of the A of 90-98wt% and 2-10wt% form (summation=100wt%).
2. the copolymer that comprises following monomeric unit:
C=styrene or C
1-3The styrene that alkyl replaces,
The D=general formula I, one or more monomers of II or III
R wherein
1, R
2And R
3Each is H atom or C
1-15Alkyl or C
6-14Aryl or C
5-12Cycloalkyl,
Copolymer is by the C of 15-95wt% and the D of 2-80wt%, the C of preferred 50-90wt% and the D of 10-50wt% and more preferably the C of 70-85wt% and the D of 15-30wt% form summation=100wt% of C and D.
3. the copolymer that comprises following monomeric unit:
E=acrylic acid, methacrylic acid or CH
2=CR-COOR ', wherein R is H atom or CH
3Group and R ' are C
1-15Alkyl or C
5-12Cycloalkyl or C
6-14Aryl,
F=styrene or C
1-3The styrene that alkyl replaces,
The G=general formula I, one or more monomers of II or III
R wherein
1, R
2And R
3Each is H atom or C
1-15Alkyl or C
5-12Cycloalkyl or C
6-14Aryl,
One or more ethylenically unsaturated monomers of H=, it can with E and/or with F and/or with the G copolymerization and be selected from α-Jia Jibenyixi, vinylacetate, acrylic compounds ester, be not styrene, vinyl ethers, isopropenyl ethers and the alkadienes that methacrylic ester, vinyl chloride, vinylidene chloride, the halogen of E replaces
Copolymer is by the E of 30-99wt%, the F of 0-50wt%, the G of＞0-50wt% and the H of 0-50wt%, the E of preferred 45-97wt%, the F of 0-30wt%, the G of 3-40wt% and the H of 0-30wt% and the more preferably E of 60-94wt%, the F of 0-20wt%, the G of 6-30wt% and the H of 0-20wt% form, and the summation of E, F, G and H is 100wt%.
4. the polymer of following monomeric unit:
R wherein
1And R
2Be by inessential atom C, H, O, S, substituting group and R that P and halogen atom are formed
1And R
2The summation of molecular weight is 40 at least.The example monomeric unit comprises acrylic acid, methacrylic acid or CH
2=CR-COOR ', wherein R is H atom or CH
3Group and R ' are C
1-15Alkyl or C
5-12Cycloalkyl or C
6-14Aryl and also be styrene and C
1-3The styrene that alkyl replaces.
The details of these material productions is described among the WO99/07927.
Especially preferably with the bead polymer form, its granularity is the additive polymer and/or the copolymer of advantageous particularly scope for purpose of the present invention.For additive polymer used according to the invention and/or copolymer, preference is as by in the melt of sneaking into fibre-forming polymer, is that the particulate forms of 0.1-1.0mm exists with the average diameter.Yet, also can use greater or lesser pearl or particle.Additive polymer and/or copolymer also can be included in the section of matrix polymer, avoid the adding of any metering.
More preferably amorphous and be insoluble to the additive polymer and/or the copolymer of polymeric matrix.They preferably have 90-200 ℃ glass transition temperature, and glass transition temperature is measured in a known way, preferably measure by differential scanning calorimetry.Further details can be from prior art, and for example from WO99/07927 identification, their disclosure clearly is incorporated herein by reference at this.
Preferably, select additive polymer and/or copolymer to make that the ratio of melt viscosity of the melt viscosity of additive polymer and/or copolymer and matrix polymer is 0.8: 1-10: 1 and be preferably 1.5: 1-8: 1.Melt viscosity uses the vibration-rheological instrument under the vibration frequency of 2.4Hz and equaling to measure under the temperature that the matrix polymer melt temperature adds 28 ℃ in a known way.For PTMT, the temperature of measuring melt viscosity is 255 ℃.Further details also can find in WO99/07927.The melt viscosity of additive polymer and/or copolymer preferably is higher than the melt viscosity of matrix polymer and determines that the selection of additive polymer and/or the concrete range of viscosities of copolymer and the selection of ratio of viscosities are of value to the performance of optimizing the yarn product.Given optimum ratio of viscosities can minimize the additive polymer of adding and/or copolymer quantity and therefore, especially, and the economy of improving one's methods.Want the blend polymer of spinning preferably to comprise 0.05-2.5wt% and more preferably 0.25-2.0wt% additive polymer and/or copolymer.
The selection of favourable ratio of viscosities provides narrow distribution and the additive polymer and/or the required fibrillar structure of copolymer in fiber of additive polymer and/or copolymer granularity in polymeric matrix.The high glass-transition temperature of comparing additive polymer and/or copolymer with matrix polymer guarantees this fibrillar structure rapidly solidified in the fiber that is spun into.Following the additive polymer after spinning head occurs and/or the maximum particle size of copolymer closely is about 1000nm, and particle mean size is 400nm or littler.Obtain favourable fibrillar structure after with tensile fiber, long filament comprises that 60wt% is with the fibril form at least, and length is that 0.5-20 μ m and diameter are additive polymer and/or the copolymer of 0.01-0.5 μ m.
But the preferred thermoplastic molding of useful polyester of the present invention and can be spun into long filament and coiling.In this context, the restriction viscosity number of particularly advantageous polyester is 0.70dl/g-0.95dl/g.
Polymer melt for example can directly be produced during melt extruding machine from the final reactor taking-up of polycondensation device or from the solid polymer section.
A kind of known way of introducing the spinning additive is to disperse equably therein to form fine particle being metered to the matrix polymer neutralization at fusion or solid form.Advantageously, can use the device of in DE 100 22 889, describing.
In the method for the invention, with the melt of polyester or melt blend by Spinning pumps under constant speed (speed by known formula calculate make obtain required fiber linear density) pumping, in the spinneret assembly to extrude by the hole in the assembly die plate to form melt filament.
Melt for example can prepare extruder from polymer chips, particularly advantageous in this case be at first with chip drying to the water content of＜30ppm with particularly arrive＜water content of 15ppm.
The temperature of melt, it is commonly referred to spinning temperature and it is measured more than Spinning pumps, depends on the polymer of use or the fusing point of blend polymer.It is preferably placed at the scope that is provided by formula 1:
Formula 1:
T
m+15℃≤T
sp≤T
m+45℃
Wherein
T
mBe polyester fusing point [℃]
T
SpBe spinning temperature [℃].
Predetermined parameter is used for limiting hydrolysis and/or thermoviscosity descends, and it should be advantageously very low.In the context of the present invention, less than 0.12dl/g with to descend less than the viscosity of 0.08dl/g especially be required.
Melt uniformity has direct influence to the performance of the long filament that is spun into.Therefore preferred the use contained at least one element and is installed in the following static mixer of Spinning pumps with the homogenising melt.
The die plate temperature, it depends on spinning temperature, by the secondary heating system control of plate.Useful secondary heating system for example comprises by " biphenyl (Diphyl) " or the other convection current or the spinning bundle of pharoid heating.The temperature of die plate is generally equal to spinning temperature.
Can obtain the temperature increase of die plate by the barometric gradient in the spinneret assembly.Known derivation, for example K.Riggert " Fortschritte in der Herstellung vonPolyester-Reifenkordgarn " 21,379 pages of Chemiefasern (1971) have described the about 4 ℃ temperature increase of per 100 crust pressure drops.
Further can be by using loose filter media control die pressure, particularly by using particle mean size to be 0.10mm-1.2mm, steel sand and/or the filter disc of preferred 0.12mm-0.75mm, it can weaving or the formation of non-woven metal fabric from fineness≤40 μ m.
In addition, the pressure drop in the die holes is influential to total pressure.Die pressure is preferably set to 80 crust-450 crust, particularly 100 crust-250 crust.
Spin journey draw ratio i
Sp, that is, withdrawal speed is to the ratio of extruded velocity, and according to US5,250,245 by the density of formula 2 from polymer or polymeric blends, and spinneret hole diameter and filament linear density are calculated:
Formula 2:
i
sp＝2.25·10
5·(δ·π)·D
2(cm)/dpf(den)
Wherein
δ=fusant density [g/cm
3]; For PTMT=1.12g/cm
3
D=spinneret hole diameter [cm]
The dawn number [den] of each long filament of dpf=.
For purpose of the present invention, spinning the journey draw ratio is 70-500, preferred 100-250.
The preferred length/diameter of spinneret hole of selecting is than being 1.5-6, particularly 1.5-4.
The long filament of extruding is by the quenching delay zone.The quenching delay zone directly is configured in below the filament spinning component as recessed area, wherein protects the long filament that occurs from spinneret hole to avoid the direct effect of refrigerating gas and during spinning Cheng Lashen or cooling, postpone.The movable part (active part) of recess is constituted the extension that filament spinning component enters the spinning bundle, make long filament surround by heated wall.Form inertia part (passive part) by the heat-insulation layer and the framework that is not heated.The length of movable recess is that the length of 0-100mm and inertia part is 20-120mm, is subject to 30-200mm, the total length of preferred 30-120mm.
As substituting of movable recess, reheater can be positioned at below the spinning bundle.With movable recess in pairs than, then this zone of cylindrical shape or rectangular cross section comprises that at least one is independent of the heating system of spinning bundle.
With one heart around spin journey under the situation of porous quench system radially, can use the cylindrical shape covering to reach quenching and postpone.
Then long filament is cooled to be lower than the temperature of solidification temperature.For purpose of the present invention, solidification temperature is that melt becomes solid-state temperature.
In the context of the present invention, determined that particularly advantageous is that long filament is cooled to their substantially no longer sticking temperature.Particularly advantageous is the crystallization temperature that long filament is cooled to they, particularly is cooled to be lower than the temperature of their glass transition temperatures.
The measure that is used for quenching or cooling long filament is known from prior art.The useful especially refrigerating gas that is to use particularly cools off air according to the present invention.The temperature of cooling air is preferably 12 ℃-35 ℃ and particularly 16 ℃-26 ℃.The speed of refrigerating gas advantageously is 0.20m/sec-0.55m/sec.
For example can use the single ended system cooling long filament that comprises single cooling tube, single cooling tube contains the wall of porous.Certainly suck the cooling that effect obtains each independent long filament by active refrigerating gas supply or by what adopt long filament.As substituting of single pipe, also can use familiar crossing current quench system.
In cooling with spin in the particular of journey drawing zone, will be exposed in length from the long filament that delay zone occurs is 10-175cm and the preferred cooling air the 10-80cm zone.Length is that the zone of 10-40cm is particularly suitable for the zone that long filament and length at each long filament of the linear density≤1.5dtex of coiling place (windup) is 20-80cm and is particularly suitable for the long filament that linear density is each long filament of 1.5-9.0dtex.Be 0.2-20 subsequently: 1, be preferably 0.4-5: 1 unwinding place air to the ratio of spinning Cheng Sudu under, spin cross-sectional configurations and sizeization in the journey throughput direction by control, with long filament and the air followed in conjunction with by having the groove that reduces cross section.
After the temperature that long filament is cooled to below the solidification point, their are restrained to form yarn beam.The conventional method that can use yarn speed and/or yarn temperature online to measure, for example use from the laser dopper flowmeter airspeedometer of TSI/ Germany or from the infrared camera of Goratec/ Germany type i RRIS 160, determine according to the present invention from the suitable distance of the convergence point of spinning head bottom surfaces.It is 500-2500mm, preferred 500-1800mm.Under the more small distance of≤1500mm, the long filament of linear density≤4.5dtex converges multifilament bundled in the time of preferably will being spun into, and under bigger distance the thicker long filament of preferred convergence.
Make by the material of low especially friction for all surface that the object of the invention advantageously preferably contacts with the long filament that is spun into.So substantially, avoid the long filament that ruptures and higher-quality filament yarn is provided.What be particularly suitable for this purpose is low-friction surface from Ceramtec/ Germany " TriboFil " specification.
Restrain long filament in the lubricator pin, it provides the spin finish of yarn aequum under even speed.Specially suitable lubricator pin is characterized as intake section, contains the yarn tube and the exit portion in hole, oil-in.Intake section is funnelform, makes to avoid by the still contact of the long filament of drying.After the providing of spin finish, the contact point of long filament occurs in the yarn fiber tube.Yarn tube and hole, oil-in meet the number of yarn linear density and long filament on width.Aperture and width at 1.0mm-4.0mm are specially suitable.The exit portion of lubricator pin is configured to the homogenising district, and it preferably includes oily storage tank.Such lubricator can for example obtain from the Ceramtec/ Germany or the Goulston/ U.S..
The uniformity that oil applies has great importance for the present invention.For example can use Rossa meter as according at Chemiefasern/Textilindustrie, determine the uniformity in the method for 896 pages of descriptions in November, 42/94,1992.Preferably, such program provides for less than 90 numerical digits (digital) and the standard deviation value that applies less than the oil of 60 numerical digits especially.For purpose of the present invention especially preferably less than 45 numerical digits with particularly apply standard deviation value less than the oil of 30 numerical digits.The standard deviation value of 90 or 45 numerical digits is respectively approximately corresponding to 6.2% or 3.1% variation coefficient.
For purpose of the present invention particularly advantageous be spin finish pipeline and pump are designed to self-purging avoiding bubble, but this is because the change perceived that bubble can cause oil to apply.
According to the present invention, particularly preferably in reel for yarn around before with filament entanglement.In the context of the present invention, the injector of finding to contain airtight yarn tube is specially suitable, and this is because such system prevents in feed well even in the buffering of low yarn tension and high air pressure yarn under working.The entanglement injector is preferably placed between the godet roller and by the friction speed of entrance and exit godet roller and controls yarn outlet tension force.Yarn outlet tension force should be no more than 0.20cN/dtex and should mainly have the numerical value of 0.05cN/dtex-0.15cN/dtex.The entanglement air pressure is a 0.5-5.5 crust, or is at most in coiling speed under the situation of 3500m/min and is at most 3.0 crust.
Preferably snarling is arrived the node counts of 10n/m at least.Do not have the interstitial position and be interested especially less than the maximum of 100cm less than 100% node counts index variation value.Advantageously, provide 〉=node counts of 15n/m greater than the employings of 1.0 crust air pressures, it be characterized as high evenness be variation coefficient be not more than 70% and maximum no interstitial position be 50cm.In actual applications, find LD type system, from Slack ﹠amp from Temco/ Germany; The dual system of the Parr/ U.S. or be useful especially from the Polyjet of Heberlein.
The peripheral speed of first Galette unit is called withdrawal speed.In the coiling assembly, the yarn silk is reeled with the package (bobbin) on the formation make-up machine before, can adopt other godet roller system.
Stable, flawless package is the basic prerequisite that the yarn zero defect is reeled and desirable zero defect is further processed.Therefore, in the context of the present invention, the coiling tension of employing is 0.025cN/dtex-0.15cN/dtex and is preferably 0.03cN/dtex-0.08cN/dtex.
According to the important parameter of the inventive method be more than the unwinding godet roller and between the yarn tension setting value.As known, by the actual orientation tension force of Hamana, form substantially by friction tension on thread-carrier and lubricator and yarn-windage tension force for this tension force.For purpose of the present invention, more than the unwinding godet roller and between yarn tension be 0.05cN/dtex-0.20cN/dtex and be preferably 0.08cN/dtex-0.15cN/dtex.
The low-tension of crossing that is lower than 0.05cN/dtex no longer provides partially oriented required degree.When tension force surpassed 0.20cN/dtex, this tension force can reeled and store in the bobbin process and induce memory effect, and it causes the deterioration of yarn parameter.
Pass through from the distance of the lubricator that sprays spinning head the length in the gap between friction surface and unwinding godet roller control tension force according to the present invention.This length advantageously is not more than 6.0m and preferably less than 2.0m, arranges that by the parallel connection structure spinning system and unwinder are to guarantee straight yarn path.
Geometric parameter also be described in convergence point and batch between yarn regulate the time.Quick loose package quality to foundation during this period is influential.The preferred adjusting time of selecting to determine like this is 50-200ms.
According to the present invention, the coiling speed of POY is 2200m/min-6000m/min.Preferred selection speed between 2500m/min-6000m/min.The blend polymer of reeling under the speed of preferred especially 3500m/min-6000m/min.
Advantageously, be≤45 ℃ by regulating the yarn package environment, particularly the relative humidity of 12-35 ℃ temperature and 40-85% is carried out the method according to this invention.Further advantageously under being wrapped in POY 12-35 ℃ and 40-85% relative humidity, further first being processed stored at least 4 hours.
Store after 4 weeks under standard conditions, long filament according to the present invention has following performance:
A) 90%-165%, the extension at break of preferred 90-135%,
B) at least 30%, the boiling water of preferred 〉=40% shrinks,
C) less than 1.1%, preferably less than 0.9% normal Wu Site,
D) birefringence of 0.030-0.058,
E) less than 1.35g/cm
3, preferably less than 1.33g/cm
3Density,
F) change≤4.5%, the fracture load coefficient of preferred≤2.5% and
G) change≤4.5%, the extension at break coefficient of preferred≤2.5%.
Term " standard conditions " is known for those skilled in the art and passes through the DIN53802 standard definition.Under " standard conditions " according to DIN 53802, it is 65 ± 2% with relative humidity that temperature is 20 ± 2 ℃.
In addition for purpose of the present invention particularly advantageous be when after directly reeling, measuring boiling water be punctured into 50-65% and under standard conditions, store be at least after 4 weeks 30% be preferably 〉=40%.Astoundingly, determined that the POY bobbin of producing in this way has excellent further processing characteristics.
The method of measuring the indication material parameter is known for those skilled in the art.They can be discerned from technical literature.Although can adopt variety of way to measure most parameter, the following method of measuring the long filament parameter can prove for the present invention seeks to particularly advantageous:
Inherent viscosity is measured in the Ubbelohde capillary viscometer and calculated by the formula of being familiar with at 25 ℃.The solvent that uses is phenol and 1,3 of 2-dichloro-benzenes: 2w/w mixture.The concentration of solution is the every 100ml solution of 0.5g polyester.
Use is measured each of fusing point, crystallization temperature and glass transition temperature from the DSC calorimeter of Mettler.With sample initial heating to 280 ℃ with its fusion and quenching then.In 20 ℃ of-280 ℃ of scopes, under the 10K/min rate of heat addition, carry out dsc measurement.Determine the temperature of report by processor.
In density gradient column, under 23 ± 0.1 ℃ temperature, measure filament density.The reagent that uses is normal heptane (C
7H
16) and tetrachloromethane (CCl
4).The result of density measure can be used for the density D with amorphous polyester
aDensity D with crystalline polyester
kBe basic calculation degree of crystallinity.It is D for the corresponding numerical value of PTMT for example that calculating is described in the document neutralization
a=1.295g/cm
3And D
k=1.429g/cm
3
Use in a known way and accurately reel and Weighing mechanism measure linear density.The pretension that uses is 0.05cN/dtex for POY advantageously and is 0.2cN/dtex for DTY.
On the Statimat device, measure fracture strength and extension at break under the following conditions: be 200mm and be the clamping length of 500mm for DTY for POY, be 2000mm/min and be the extension speed of 1500mm/min for POY, be 0.05cN/dtex and be the pretension of 0.2cN/dtex for DTY for POY for DTY.With the maximum breaking load value divided by linear density to determine fracture strength and under peak load, to measure extension at break.
By in 95 ± 1 ℃ water, under tension-free state, handle long filament reeled yarn 10 ± 1min and measure boiling water and shrink.By being 0.05cN/dtex for POY and being to reel under the pretension of 0.2cN/dtex to prepare reeled yarn for DTY; Before under 0.2cN/dtex, heat-treating and reeled yarn linear measure longimetry afterwards.The difference of length is used for calculating in a known way boiling water and shrinks.
Birefringence is by at DE 19,519, and the method for describing in 898 is measured, and the disclosure of the document clearly is incorporated herein by reference at this.
According to DIN 53840 parts 1, use Texturmat device from Stein/ Germany, under 120 ℃ colour developings (development) temperature, measure the creep parameters of modified continuous filament.
Normal Wu Site numerical value uses the 4-CX uster tester to measure and be reported to Wu Site % numerical value.Test speed is that 100m/min and testing time are 2.5min.
According to POY of the present invention simply with further processing, particularly stretcher strain.In the present invention, stretcher strain is preferably being carried out under the deformation velocity of 500m/min at least and under the deformation velocity particularly preferably in 700m/min at least.Draw ratio preferably was at least 1.35: 1 and particularly at least 1.40: 1.Particularly advantageous is in the high temperature heater (HTH) type machine, for example from stretcher strain on the AFK machine of Barmag.
In this way the bulk filament of Sheng Chaning demonstrate low number of defects and under boiling in when adopting DISPERSE DYES not have carrier dyeing, the depth of color of excellence and the uniformity of color.
Varicosity SET long filament produced according to the invention preferably has greater than the fracture strength of 26cN/tex with greater than 36% extension at break.Under varicosity HE long filament situation, it can not have the heat treatment of secondary heater and obtains, and fracture strength is preferably greater than 26cN/tex and extension at break greater than 30%.
The body of long filament and elastic behavior excellence according to the present invention.
More particularly describe illustrative embodiment of the present invention now, the present invention is not limited to this embodiment.
Embodiment 1-3
Spinning and coiling
With inherent viscosity is 0.93dl/g, and melt viscosity is 325Pas (measuring down 2.4Hz and 255 ℃), and fusing point is 227 ℃, and crystallization temperature is that 72 ℃ and glass transition temperature are that 45 ℃ PTMT section is at the water content of 130 ℃ of following tumble dries to 11ppm.
With section fusion in, make that the temperature of melt is 255 ℃ from the 3E4 extruder of Barmag.This melt is joined in the Plexiglas 7N polymethyl methacrylate from the difference amount of R hm GmbH/ Germany as the extensibility reinforcing agent, and this polymethyl methacrylate has been dried to the residual moisture content less than 0.1%.
For this purpose, with additive polymer fusion in melt extruding machine, the use gear wheel metering pump is fed to feeding mechanism and from then on delivers in the polyester components by the injection nozzle in the flow direction.With two kinds of melt homogenising and in from the SMX static mixer of Sulzer fine dispersion, static mixer contains 15 elements and internal diameter is 15mm.
The melt viscosity of Plexiglas 7N is 810Pas (2.4Hz, 255 ℃), and the result is that the ratio of additive and polymer malt viscosity is 2.5: 1.
The conveying capacity of melt is 63g/min, and the time of staying is that 6min and adjusting make that to the metered amounts of spinneret assembly the POY linear density is about 102dtex from Spinning pumps.Use various winding speed setting values.To be that an element of the HD-CSE type static mixer of 10mm is installed in below the Spinning pumps, but enter more than the point of spinneret assembly from the Fluitec internal diameter.The secondary heating system that will be used for product pipeline and spinning piece (it comprises pump and spinneret assembly) is set to 255 ℃.Spinneret assembly comprise highly for the 350-500 μ m steel sand of 30mm and same 20 μ m weaving filter devices and 40 μ m woven filter as filter media.Is that 0.25mm and length are that the 80mm diameter spinneret plate in 34 holes of 1.0mm is extruded with melt by comprising diameter.Die pressure is 120 crust.
Quenching delay zone length is 100mm, by the 30mm in heated wall and insulation and not the 70mm in the heating frame form.Adopt horizontal flow to cross melt filament and spin the air quenched of journey 1500mm length.The flow rate of quench air is 0.35m/sec, and it is 80% with relative humidity that temperature is 18 ℃.Long filament about 800mm place below spinning head becomes solid.
Be positioned at from the yarn lubricator of spinning head 1050mm distance and be used for before convergence, providing spin finish to the end.Lubricator has the TriboFil surface and diameter is the inlet opening of 1mm.The amount of the spin finish that applies is 0.40%, based on fibre weight.
The journey of spinning that will restrain is then delivered to up-coiler.Distance between the lubricator and the first unwinding godet roller is 3.2m.The adjusting time is 105-140ms.A pair of godet roller is twined by yarn S.Between godet roller is Temco entanglement injector, and it uses the air-operated of 1.5 bar pressures.According to speed setting, the coiling speed of setting Barmag SW6 up-coiler makes that batching yarn tension is 5cN.Indoor conditions is adjusted to 24 ℃ and 60% relative humidity makes that the result is that temperature in yarn package is about 34 ℃.
Obtain the remarkable increase of productivity ratio for all adding amount of additives.The 10kg bobbin of producing is removed from winding mandrels easily.The remarkable part of POY yarn that obtains is to store the good time constancy of yarn property in 4 weeks under the standard conditions of DIN 53802 definition.Find that directly the boiling water after spinning and coiling is punctured into 51-54%.Deformability that discovery reaches and dye uniformity excellence.For the POY speed of using, the draw ratio that use is high astoundingly.
Other parameter and performance data see Table 1-4.
Table 1: test parameters
| Test parameters | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Additive concentration | [％] | 0.5 | 0.7 | 1.0 |
| Withdrawal speed | [m/min] | 3011 | 3520 | 4022 |
| Coiling speed | [m/min] | 3005 | 3500 | 4000 |
| Spin the journey ratio of elongation | 183 | 182 | 181 | |
| Yarn tension | ||||
| More than godet roller 1 | [cN] | 13 | 15.5 | 16 |
| Between godet roller 1max | [cN] | 12 | 13 | 12.5 |
| More than godet roller 2 | [cN/dtex] | 0.13 | 0.15 | 0.16 |
| Between godet roller 2max | [cN/dtex] | 0.11 | 0.13 | 0.12 |
| Yarn tension 1 | [cN] | 6.3 | 5.9 | 6.4 |
| Yarn tension 2 | [cN/dtex] | 0.062 | 0.058 | 0.062 |
1: absolute
2: based on linear density
The material property of table 2:PTMT POY long filament
1
| Material property | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Linear density | [dtex] | 102 | 102.5 | 103 |
| Fracture strength | [cN/dtex] | 20.2 | 21.8 | 22.3 |
| Extension at break | [％] | 132.7 | 115.4 | 98.2 |
| Normal Wu Site | [％] | 0.80 | 0.90 | 0.94 |
| Boiling water shrinks | [％] | 48 | 44 | 38 |
| Birefringence 10 3 | Δn | 36 | 47 | 51 |
| Density | [g/cm 3] | 1.315 | 1.318 | 1320 |
| Fracture load CV | [％] | 1.7 | 1.5 | 2.1 |
| Extension at break CV | [％] | 1.9 | 1.9 | 3.3 |
CV: variation coefficient
1: store under normal operation and measure after 4 weeks
Stretcher strain
PTMT long filament bobbin was stored for 4 weeks and delivered to Barmag FK6-S-900 draw texturing machine then under as the standard conditions of DIN53802 definition.Be used for stretcher strain with the test parameters of producing the SET long filament see Table 3 and the material property of the varicosity SET long filament that obtains see Table 4.
Use the UNITENS system of Barmag under following limits value is set, to measure deformation defect: UP/LP=3.0cN, UM/LM=3.0cN.
Table 3: the test parameters of stretcher strain
| Test parameters | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Speed [m/min] | [m/min] | 700 | 700 | 700 |
| Draw ratio | 1∶1.70 | 1∶1.60 | 1∶1.44 | |
| The D/Y ratio | 2.1 | 2.1 | 2.1 | |
| Heater 1 temperature | [℃] | 155 | 155 | 155 |
| Heater 2 temperature | [℃] | 160 | 160 | 160 |
| The stretching defective | [n/10kg] | 0 | 0 | 0 |
| Yarn tension | ||||
| F 1, more than assembly | [cN] | 17 | 18 | 19 |
| F 2, below assembly | [cN] | 19 | 21 | 21 |
| F 2-CV | [％] | 0.78 | 0.93 | 0.89 |
F
2-CV:F
2Variation coefficient
Table 4: the material property of stretcher strain long filament
| Material property | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Linear density | [dtex] | 67 | 69 | 79 |
| Fracture strength | [cN/dtex] | 26.9 | 29.6 | 28.2 |
| Extension at break | [％] | 38.6 | 37.8 | 38.0 |
| Can chromaticly observe | Evenly | Evenly | Evenly | |
| The creep rigidity | [％] | 84 | 85 | 79 |
| Creep is shunk | [％] | 25 | 24 | 23 |
Claims (10)
1. produce and reel for one kind, be not less than the method for the polybutylene terephthalate (PBT) of 90wt% and/or polytrimethylene-terephthalate's POY polyester filament, it is characterized in that this method comprises based on the polyester filament gross weight:
A) spin the journey draw ratio in the setting of 70-500 scope,
B) will be directly from the long filament in spinning head exit length by quenching delay zone 30mm-200mm,
C) long filament is quenched to below the solidification temperature,
D) long filament is restrained in the distance from spinning head bottom surfaces 500mm-2500mm,
E) be set in the unwinding godet roller above and between yarn tension be 0.05cN/dtex-0.20cN/dtex,
F) under the yarn tension of 0.025cN/dtex-0.15cN/dtex, batch yarn,
G) setting coiling speed is 2200m/min-6000m/min,
H) and in mixture use based on the long filament gross weight, comprise the polyester of the additive polymer extensibility reinforcing agent of 0.05wt%-2.5wt%.
2. the method for claim 1 is characterized in that using polybutylene terephthalate (PBT) and/or the polytrimethylene-terephthalate of restriction viscosity number as 0.7dl/g-0.95dl/g.
3. claim 1 or 2 method is characterized in that batching by the temperature of≤45 ℃ of settings in around yarn package.
4. claim 1 or 2 method is characterized in that in further first being processed the POY bobbin being stored 4 hours under 12-35 ℃ and 40-85% relative humidity at least.
5. claim 1 or 2 method is characterized in that coiling speed is set at 2500m/min-6000m/min.
6. the POY polyester filament that can obtain by at least one method in the aforementioned claim, it has following performance after it is characterized in that storing for 4 weeks under the standard conditions of definition in DIN 53802:
A) extension at break of 90%-165%,
B) at least 30% boiling water shrinks,
C) less than 1.1% normal Wu Site,
D) birefringence of 0.030-0.058,
E) less than 1.35g/cm
3Density,
F) change≤4.5% fracture load coefficient and
G) the extension at break coefficient of variation≤4.5%.
7. the POY polyester filament of claim 6 is stored the density of 4 all these polyester filaments afterwards less than 1.33g/cm under the standard conditions that it is characterized in that defining in DIN 53802
3
8. method of producing the varicosity polyester filament is characterized in that in draw texturing machine in the speed and 1.35 of 500m/min at least at least: under 1 the draw ratio, the long filament of claim 6 or 7 is processed into bulk yarn.
9. the varicosity polyester SET long filament that can obtain by the method for claim 8, the fracture strength that it is characterized in that them greater than 26cN/tex and extension at break greater than 36%.
10. the varicosity polyester HE long filament that can obtain by the method for claim 8, the fracture strength that it is characterized in that them greater than 26cN/dtex and extension at break greater than 30%.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10054422 | 2000-11-03 | ||
| DE10054422.3 | 2000-11-03 |
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|---|---|
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| CNB018102972A Expired - Fee Related CN1210449C (en) | 2000-11-03 | 2001-11-02 | Method for spinning and winding of polyester filaments using spinning additives, polyester filaments obtained by spinning method, draw texturing of polyester filaments and bulked polyester filaments |
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| JP3910038B2 (en) * | 2001-10-18 | 2007-04-25 | 旭化成せんい株式会社 | Pre-oriented yarn package and manufacturing method thereof |
| 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 |
| KR20040094688A (en) * | 2002-02-12 | 2004-11-10 | 짐머 악티엔게젤샤프트 | A process for the production and for the winding of polyester multi-filament yarns as well as the polyester multi-filament yarns obtainable by said method and a device for the winding of one or more multi-filament yarns |
| DE10213921B4 (en) * | 2002-03-28 | 2006-10-12 | Röhm Gmbh | A method of spinning and winding polyester multifilament yarns using spin additives and polyester multifilament yarns obtainable by the spinning process |
| TW200741049A (en) * | 2005-12-27 | 2007-11-01 | Shell Int Research | Polyester yarn and process for producing |
| CN113481624B (en) * | 2021-06-24 | 2023-04-28 | 杭州惠丰化纤有限公司 | Polyester yarn and production process thereof |
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| US3975488A (en) * | 1972-10-24 | 1976-08-17 | Fiber Industries, Inc. | Process for preparing poly(tetramethylene terephthalate) yarn |
| TR200000316T2 (en) * | 1997-08-05 | 2001-07-23 | R�Hm Gesellschaft M�T Beschrankter Haftung | Process for processing polymer blends in filaments. |
| JPH11172526A (en) * | 1997-11-26 | 1999-06-29 | Asahi Chem Ind Co Ltd | Polyester fiber having low thermal stress and spinning thereof |
| JP3249097B2 (en) * | 1999-07-12 | 2002-01-21 | 旭化成株式会社 | Polyester fiber suitable for false twisting and manufacturing method |
| TW522179B (en) * | 1999-07-12 | 2003-03-01 | Asahi Chemical Ind | Polyester yarn and producing method thereof |
| US6287688B1 (en) * | 2000-03-03 | 2001-09-11 | E. I. Du Pont De Nemours And Company | Partially oriented poly(trimethylene terephthalate) yarn |
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