CN1179074C - Poly (trimethylene) terephthalate textile staple production - Google Patents
Poly (trimethylene) terephthalate textile staple production Download PDFInfo
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- CN1179074C CN1179074C CNB018082173A CN01808217A CN1179074C CN 1179074 C CN1179074 C CN 1179074C CN B018082173 A CNB018082173 A CN B018082173A CN 01808217 A CN01808217 A CN 01808217A CN 1179074 C CN1179074 C CN 1179074C
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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
- D01F6/58—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
Abstract
A process for making textile staple fibre from polytrimethylene terephthalate (PTT) which comprises: (a) melt extruding PTT polymer at 245 to 253 DEG C, (b) spinning the extruded PTT into yarn using at least one spinneret, (c) moving the spun yarn to a first takeup roll wherein the distance from the spinneret to the roll is from 16 to 20 feet, (d) cooling the spun yarn to less than 31 DEG C. before it reaches the roll, (e) prior to the draw process, preconditioning the yarn under tension at a temperature of at least 60 DEG C, (f) drawing the yarn at a temperature of at least 60 DEG C, (g) allowing the drawn yarn to relax at a temperature of up to 190 DEG C, and (h) crimping the drawn yarn at a temperature of 70 to 120 DEG C, and decreasing the drawn yarn feed denier into the crimper by 10 to 60 percent by denier.
Description
Invention field
Polytrimethylene terephthalate is to be suitable for the new polyester resin that carpet, textiles and other thermoplastic resin are used.From chemically, polytrimethylene terephthalate (PTT) is by 1, the aromatic polyester resin that ammediol (PDO) and terephthalic acid (TPA) polycondensation are made.Preparing textile staple (staple) by PTT can carry out on multiple industrial processing equipment.
Background of invention
The two-step method that the preparation of PET synthetic staple normally separates.The first step relates to extrudes not stretch yarn, this not stretch yarn be saved for second the step stretched operation.The drawing process that is used for the staple fibre preparation mainly contains two kinds: stretch-lax and stretching-heat treatment.So how the main distinction of these two kinds of methods carries out filament contraction.In stretching-lax staple fibre preparation method, shrinking strategy is to curl in baking oven fiber to be retracted to desired properties in advance afterwards.In stretching-heat treatment staple fibre preparation method, shrinking strategy is to add thermal fiber, makes it to carry out the constant length crystallization before curling.
People have prepared staple fibre by polyethylene terephthalate (PET), and this method is very ripe.Therefore, hope can prepare the PTT staple fibre on existing equipment.Yet, between these two kinds of polymer many differences are arranged, be difficult to maybe can not make PTT on existing staple fibre production equipment, to make the useful staple fibre of industry thus.For the ease of understanding is how to prepare the PTT staple fibre on existing equipment, and we need mention several technologic problems:
How to characterize the not tensile property of stretch yarn? is the tensile property of stretch yarn not how along with the time changes? this is described in embodiment 1.
How in extrusion, to control the not performance of stretch yarn? this is described in embodiment 2.
Is what not the general tensile property of stretch yarn? this is described in embodiment 3 and 4.
Is not how controlling fiber shunk in stretch yarn preparation and the storage process? this is described in embodiment 5.
How staple fibre stretch and final staple fibre product in controlling fiber shrink? this is described in embodiment 6.
Does how the crimped fibre commercial run that makes it to be used in the downstream staple fibre weaving spun yarn and bondedfibre fabric provide structure and cohesive force? this is described in embodiment 7.
The how Young's modulus and the tensile property of heat setting and control staple fibre.What influence is the staple fibre performance have to the spun yarn performance; This is described in embodiment 8.
What the basic skills of preparation staple fibre is on existing equipment, and this method will be mentioned the complementary character of above-mentioned six technological problemses.The present invention just provides a kind of like this method.
Summary of the invention
The invention describes the two step staple fibre preparation methods of a kind of PTT of utilization.The first step is to extrude not stretch yarn (UDY).In second stretching step, change UDY into the staple fibre product.
According to the present invention, providing a kind of prepares in the equipment at existing PET textile staple, the method for preparing textile staple by polytrimethylene terephthalate (PTT), comprise (a) 245 ℃-253 ℃, melt extrude the PTT polymer under preferred 245 ℃-250 ℃, (b) utilize at least one spinning plate with the PTT spun yarn of extruding, (c) spun yarn is moved to first take up roll, wherein the distance between this roller and the spinning plate is the 16-20 foot, (d) spun yarn was cooled to be lower than 31 ℃ before arriving first take up roll, preferably be lower than 25 ℃, most preferably be lower than 20 ℃, (e) randomly, spun yarn is stored in temperature is no more than 31 ℃, that weather has been controlled is indoor (this step and previous step rapid the two be used to minimize the not early-age shrinkage of stretch yarn before stretched operation), (f) before the stretched operation, at at least 60 ℃, under preferred 60-100 ℃, this yarn of preconditioning under tension force, (g) at least 60 ℃, preferred 60-100 ℃ of following drawing, randomly preferably carrying out second stretches, wherein total major part that stretches occurs in first stretching, preferred total 80-85% that stretches occurs in first stretching, wherein second and being stretching in subsequently be higher than the actual maximum point of first draft temperature to the fusing point of yarn, preferred 60 ℃-160 ℃, most preferably carry out under 80 ℃-100 ℃, (h) in order to increase the initial Young's modulus of drawing, make drawing up to 190 ℃, it is lax under preferred 100-140 ℃ that (relaxation rate can be 2-25%, perhaps can be higher, but be preferably 2-10%), if (i) carry out relaxation step, just at 70 ℃-120 ℃, curling drawing under preferred 80-120 ℃, if do not carry out relaxation step, just under 70-100 ℃, and in crimping machine, the feeding dawn number of drawing is reduced the 10-60% dawn, the preferred 40-60% dawn by the drawing feeding speed of the corresponding PET staple fibre of preparation in this existing equipment.Also have, additionally or in combination, the crimping machine volume that is used to prepare PET in the volume ratio existing equipment of crimping machine increases 10-50%, preferred 20-35%.Preferably, the selection of condition is based on specific equipment and required productive rate.
Brief Description Of Drawings
Now, the present invention will be described by embodiment with reference to following accompanying drawing, wherein:
Fig. 1 is the sketch of the method step of the packing fiber that will be described from resin to its key factor.
Fig. 2 is the intensity elongation profile of equilibrium, helps the possible range near PTT staple fibre performance.
Fig. 3 is the stresses typical/strain curve of expression spun yarn bundle.
Fig. 4 is the influence of expression extrusion temperature to tensile fiber.
Fig. 5 represents that not the shrinkage factor of stretch yarn in different temperatures water is the function of stretch yarn spinning condition not.
Fig. 6 is an orientation maps of describing the filament contraction effect.
Fig. 7 is expression stretch bath temperature and the influence of total orientation parameter to boiling water shrinkage.
Fig. 8 is expression stretch bath temperature and the influence of total orientation parameter to 125 ℃ of xeothermic contractions.
Fig. 9 is expression stretch bath temperature and the influence of total orientation parameter to 140 ℃ of xeothermic contractions.
Figure 10 is expression stretch bath temperature and the influence of total orientation parameter to 175 ℃ of xeothermic contractions.
Figure 11 is expression stretch bath temperature and the influence of total orientation parameter to 197 ℃ of xeothermic contractions.
Figure 12 is the influence to the stretched operation coefficient of relaxation of expression draw ratio and stretch bath temperature.
Figure 13 represents that for 1.4 total orientation coefficient and the 75 ℃ of stretch bath temperature that freely relax, predetermined xeothermic contraction is the function of drier (rarefactor) oven temperature.
Figure 14 represents that for the 100%PTT yarn, the yarn of rarefactor oven temperature and application stretches to the influence of 175 ℃ of xeothermic contractions.
Figure 15 represents that for the 100%PET yarn, the yarn of rarefactor oven temperature and application stretches to the influence of 175 ℃ of xeothermic contractions.
Figure 16 is illustrated under two yarn heat setting temperatures, and 175 ℃ of xeothermic contractions of PTT and PET spun yarn are compared.
Figure 17 is the PTT that represents for 50: 50: cotton yarn, the yarn of rarefactor oven temperature and application stretches to the influence of 175 ℃ of xeothermic contractions.
Figure 18 is illustrated under two heat-set temperature, the boiling water of PTT and PET spun yarn is shunk compare.
Figure 19 is illustrated under two yarn heat setting temperatures, and the load under 5% strain of PTT and PET spun yarn is compared.
Figure 20 is illustrated under two spun yarn heat-set temperature, and percentage stress decaies in 2 minutes of PTT and PET spun yarn are compared.
Figure 21 is illustrated under two spun yarn heat-set temperature, the percentage strain of PTT and PET spun yarn is recovered (stretching in 2 minutes) and compares.
Detailed Description Of The Invention
It is feasible utilizing existing equipment to prepare polymer weaving staple fibre.Because the equipment difference that different company uses is very big, therefore carry out there are differences in this method how.In case staple fibre manufacturer makes its equipment only be fit to the special performance of PTT, so just can prepare the multiple staple fibre product that is applicable to spun yarn and bondedfibre fabric.Textile staple by PTT preparation has excellent bulkiness and drapability, therefore has compatibility in soft, bulk, the mixture, is easy to nurse and the shape-retaining ability of textiles.
1.0
Polymeric material
1.1 resin transfer and drying
The dust that the low energy air conveying system will form when cask, process equipment and storage facilities are carried resin minimizes.Before extruding, should be with the PTT resin drying to 50ppm or lower constant humidity.The influence that this humidity specification is degraded the resin that causes owing to hydrolysis in the melt spinning process minimizes.The multiple industrially drying device of dry air that utilizes can successfully satisfy this requirement.Molecular sieve (13X ﹠amp is installed; 4A), the drier of vacuum systems and lithium chloride drier can satisfy industrial humidity requirement.If possible, preferably utilize the 13X molecular sieve, be heated to 130 ℃ dry air (dew point-40 ℃ or lower) with dry 4-6 hour of polymer.When from drier, being transported to dried resin in the extruder,, utilize dry air to be absolutely necessary in order to minimize the hydrolysis in the melt spinning process.
In big industrially drying device, dry PTT is controversial with the speed synchronous with extruding output.Like this, need higher baking temperature.The air themperature of PTT drier should be above 165 ℃.When utilizing 165 ℃ of air, the drier time of staying should be above 4 hours.
1.2 stretch yarn (UDY's) does not extrude
Typical melt preparation system comprises extruder, spinning beam of a loom (spin beam), Melt Pump and filament spinning component.Key is to realize uniform, optimized polymer malt viscosity by minimizing the melt temperature and the time of staying.Not only can but also can carry out the industrial preparation of PTT UDY with single screw extrusion machine with twin-screw, this point is clear and definite.In double screw extruder, the excessive shear degraded for fear of polymer melt may reduce 25-50% (with respect to the PET condition) with extrusion machine fused mass pressure.During the industrial preparation of PTT UDY, the extrusion machine fused mass temperature is 245 ℃-270 ℃.For fear of the excessive degradation of polymer melt and the excessive reduction of UDY performance subsequently, must be careful when preparing PTT UDY under the melt temperature between 260 ℃-270 ℃.For PTT, optimum staple fibre melt extrusion temperature is 245 ℃-253 ℃, preferred 245 ℃-250 ℃.In the future, the PTT resin that inherent viscosity is lower may need lower temperature.Fig. 4 represents, when at 250 ℃ rather than during at 240 ℃ or 260 ℃ of following extruded polymers, obtained draftability preferably.
2.0
The not spinning of stretch yarn (UDY)
2.1 spinning beam of a loom, pump and assembly
The test that utilizes one pack system and bi-component extrusion system to prepare PTT staple fibre UDY is successful.The Spinning pumps volume and the revolution speed control system that are used for PET satisfy the low thruput of needed each position of PTT staple fibre usually.Filter medium should have the minimum aperture size of 30 μ m.In general, the industrial spinning assembly uses the filter medium of minimum.At exploitation PTT staple fibre preparation method's commitment, preferably use the medium/mistake filter sand (course sand) (90/120 order) of standard filter depth.Inhomogeneity evaluation will help to determine that filament spinning component filters or whether the extrusion system melt pressure needs to optimize to filament diameter.
The staple fibre extrusion system is resin viscosity, throughput, melt temperature and the time of staying that is designed for particular range.Usually, the needed hole of preparation PTT staple fibre throughput is than the low 20-30% of the PET product that is used for similar dawn number.This has increased the time of staying of the PTT that extrudes with PET staple fibre production equipment in fact.If melt temperature is higher than 260 ℃, this increase of melt residence time can cause degraded.If possible, feed-line and spinning beam of a loom heating system will equal extruder output polymer temperature.
2.2 spinning plate
Target product dawn number is depended in the selection of spinning plate, and is that the limited throughput of the every hole per minute by being used for stablizing melt spinning is determined.Usually, the PTT staple fibre can use the standard P ET spinning plate as the similar products design.Yet when comparing with the preparation of PET staple fibre, the PTT staple fibre need be used for the littler capillary diameter that the low dawn counts product usually.For circular cross-section, according to the melt extrusion condition, the upper limit shear rate of PTT resin is 7500-9000s
-1
The spinning plate that based target staple fibre product dawn number is selected is illustrated in the Table I.
Table I: spinning plate is selected figure
| During 1100/min, the thin dawn is counted scope | 1.0-1.3dpf | ?1.30-1.75dpf | ?1.40-1.85dpf |
| Spinning plate diameter (mm) | 0.23 | ?0.25 | ?0.35 |
| Spinning plate l/d | 1.85 | ?1.85 | ?1.85-2.0 |
| Limited throughput/hole | 0.32 | ?0.41 | ?0.45 |
It is important utilizing long fiber summit (culmination) district (spinning plate is to the distance between the take up roll).This expression, this zone should be the 16-20 foot rather than is used for the standard 8-12 foot of PET.The shrinkage factor of PTT UDY is quite high in technology, so this method must allow all long filaments to become altogether before the big stretched operation feeding yarn, and fiber can be set up stable molecular structure.In preparation PET staple fibre, this is not a subject matter.PTT has more flexible crystallization configuration, and therefore longer fiber apex region helps to stablize yarn, makes manufacturer avoid extra air conditioning expense.
2.3 quenching
Utilize crossing current and radially the trial of quench system be successful.Existing have the radially quench system of air-flow from outside to inside successfully to be used from inside to outside again.Fibre bundle is quenching quickly and evenly, to prevent the contraction of UDY in the spinning charging-tank.Although preferred quench temperature is 8-25 ℃, already used quench temperature is 8-35 ℃.Usually, the operability of the thread (thread path) by UDY limits the flow velocity of quench air.The number of filaments of each position is 350-3500 threads/position.In staple of thin denier preparation,, can have up to 6250 threads/position in modern times radially under the quench system.The optimization of quench system comprises determines that what condition can make target UDY bobbin cradle performance have best operability and the highest percentage percentage elongation.
2.4 spinning arrangement
In this specification, staple fibre extrude with the stretched operation process in all coating of being coated on the ptt fiber all be defined as spin finish.Spin finish is the fiber coating that lubricity, cohesive force and additive protectiveness are provided for ptt fiber in staple fibre preparation and downstream process.In the preparation process of PTT staple fibre, many components phosphate and mineral oil based finishing agent have successfully been used.Verified PET spin finish chemicals and painting method also are used for initial p TT staple fibre product satisfactorily.Subsequently, can change the prescription and the painting method of spin finish according to client to the feedback of staple fibre processing.
2.5 reel
The winding speed that uses in the industry PTT UDY preparation is 900-1250m/min.In the research equipment, the winding speed of UDY is 500-2250m/min.Before falling into the silk tube, it is useful that the lax of control arranged between coiling capstan winch roller and sunflower floral whorl.In order to minimize the contraction of UDY in the silk tube, it is necessary in single position all long filaments being cooled to be lower than 25-30 ℃.
3.0
Tow stretches and arrangement
3.1UDY storage
Under conventional condition of storage, PTT UDY has finished in 8 hours of extruding and has surpassed 90% maturing process.The UDY tensile property is stable in 24 hours, and after constant temperature stored 2-4 month down, tensile property did not have significant change.PTT UDY has more at low temperatures than PET UDY and shrinks tendency.Because the condition of storage that is higher than 25-30 ℃ is easy to cause UDY and shrinks, therefore should avoid.Be PTT UDY bobbin cradle to be stored in the environment of air conditioning, ideally to help avoid contraction.Cause that definite temperature that PTT UDY shrinks depends on that UDY extrudes, quenching, coiling and condition of storage.Even PTT UDY shrinks, also can seldom influence in the stretched operation process of product quality, change this UDY into one-level industry staple fibre product.
3.2 bobbin cradle size
The bobbin cradle size of PTT staple fibre is determined by the crimping machine size.In general, because ptt fiber has higher bulkiness, the bobbin cradle size that therefore is used for the PTT staple fibre is approximately 60% of PET staple fibre product.600,000 dawn drawn tows will feed in the high crimping machine of the wide 20mm of 110mm satisfactorily.This will change greater than 100-130m/min along with the increase and/or the increase of stretching throughput rate of crimping machine size.Because most of stretching production lines have the maximum line velocity of 250-300m/min, therefore increasing the crimping machine casing long-pending is another approach that improves the online productivity ratio that stretches.
3.3 the preparation of bobbin cradle and tow
Before the UDY tow being placed under the even roller tension force, avoid PTT UDY is heated to above 25 ℃.This will minimize the contraction of PTT in the feeding stretched operation, and the maintenance uniform fibers tension force of being had a few on tow cross-sections in drawing process.If do not control, can not carry out uniform UDY and shrink, the variation of orientation will limit the uniformity of stretched operation between tube and the tube.
Preferably before stretching, have pre-wetted to bathe, but its temperature can not surpass 25 ℃, unless provide driven roller and nip rolls (nippedroll) to minimize the tension force in stretching feeding stage.If there is not driven roller, this bath should be possible lowest evenness temperature.
3.4 drawing process
The PTT staple fibre stretching-prepares in the lax and stretching-heat treatment method.In stretching-relaxation method, with staple fibre heat treatment and under zero tension force drying reduce contraction.This method prepared be suitable for the PTT spun yarn and with the low modulus fiber low modulus fiber that mixes of wool fibre and acrylic fiber for example.Stretching-heat treatment method be under high-tension on roller the heat treatment tow, made and be fit to the high modulus fibre that mixes with artificial silk, cotton or other high modulus fibre on a small quantity.
In first draw stage, the incipient extension of UDY tow is selected and should be heated to minimum 60 ℃ at water, and preferred 60-100 ℃ takes place down.Keep the drawing point heating to improve the drawing process performance to the influence of producing draw ratio by remarkable reduction extrusion condition.If desired, the temperature of second draw stage is higher than the temperature of first draw stage, up to the actual peak of yarn fusing point, and preferred 60-160 ℃, most preferably 80-100 ℃.Different with PET, PTT can not become coarse in the stretch bath of heating.Other drawing zone is dispensable, has increased total mechanical draw ratio usually slightly.The phase I that main draw ratio should stretch.
Lax or heat treatment has the lax PTT staple fibre tow of 3% roller by one group of 100-130 ℃ of calender, will make the initial modulus of final PTT staple fibre increase 12-14%.This method has prepared and has been suitable as the high modulus fibre that PTT spun yarn and, artificial silk for example cotton with high modulus fibre and PET mix.When the relaxation rate by the roller group remained on 3%, from 130-150 ℃, per 10 ℃, initial modulus increased about 4%.Heat treatment PTT tow may need to increase lax by calender more than 150 ℃, to avoid too much filament breakage.Spin finish utilizes dipping bath or front/rear kiss rall to apply normally before the stage of curling, and compensates the spin finish that loses in the stretched operation.
3.5 curl
Compare with the PET tow, the PTT tow is very easy to crooked, and the bending modulus that it is low has been described.This low modulus also makes PTT have excellent feel and flexibility.In addition, PTT is more bulk than PET far away.Low bending modulus and high bulkiness require to do following change in curling condition:
● reduce dance roller and crimping machine roller, with the curling geometry of better control.
● because therefore the higher bulkiness of PTT must reduce to feed the dawn number of tow or increase the crimping machine volume.The increase of PTT bulkiness can reduce the most preferably 10-60% dawn by the tow total denier that will feed in the crimping machine, and the preferred 40-60% dawn is resolved.Another kind method is the volume increase 10-50% volume with crimping machine, preferred 20-35% volume.Also have, also can use the combination of these two kinds of methods.
● be that the nozzle that is equipped with steam and spin finish on the crimping machine is controlled the crimper temperature better ideally.
● the accuracy of improving pressure and temperature control in the crimper is necessary.
In crimper, be at least 85 ℃, when case mouth (gate) pressure is 300kPa (3bar), improved curling stability and coiling significantly.Compare with similar PET staple fibre, crimp frequency is higher, and crimp amplitude is lower.Curling stability and coiling are improved along with the increase of crimping machine temperature.Because along with the increase of curling stability, fibre cohesion increases, this will increase the defective in the carded, so crimping machine can not be heated De Taigao.
3.6 drying, shearing and packing
Lax (drying) PTT staple fibre in conventional belt baking oven, this point is clear and definite.Yet when oven temperature was elevated to the maximum temperature that is higher than in the stretched operation of front, curl geometry and shrinkage characteristic changed.In the lax staple fibre that stretches was produced, with the increase of dryer temperature, the xeothermic contraction of staple fibre and spun yarn subsequently reduced.
In stretching heat treatment staple fibre is produced, utilize lax baking oven as drier.Air velocity is high relatively, and air themperature low relatively (75-90 ℃) promotes the tow drying.These conditions do not have heat to staple fibre being relaxed or curling geometry changes.In industrial production, utilize do not transform rotary and send western Fick (tow) converter (pacificconverter) type cutting machine to shear the staple fibre tow.In commerical test, the staple fibre baling press that utilizes gravity and air to carry is packed the PTT staple fibre.
4.0
Be used for 1.7,2.5 and 3.33dtex (1.5,2.25, and 3dpf) staple fibre one Well matched side
The prescription of three kinds of typical staple fibre products is listed in the following table briefly.The production equipment of every kind of staple fibre is different.Usually need on industrial production line, attempt determining for 2-3 time the commercial run of PTT staple fibre.These prescriptions are developed on the back yard industry production equipment.Along with this method expands on the bigger equipment and higher productivity ratio, they can do a small amount of change.UDY is that the speed with 1100m/min is produced under 253 ℃ melt temperature.In order to obtain these draw ratios, need uniform extrusion condition, on all spinning stations so that the coefficient of variation of filament diameter is 3-5%.In addition, these draw ratios are to obtain on the modern production equipment of very strict control.On older equipment, the 75-85% that only reaches these draw ratios neither be abnormal.
Prescription in the Table II is also produced the prescription that staple fibre dawn number discloses a kind of high and low contraction for each target.When the phase I, the stretch bath temperature was higher than 60 ℃, the amount of contraction of draw stage significantly reduced.In addition, the draw stage amount of contraction reduces little along with draw ratio increases.When utilizing calender to come heat treatment of fibre, in crimping machine and drier, the shrinkage factor that finally stretches also further reduces.The industrial stretching throughput rate that has used 100-130m/min, and developed rate of extension up to 225m/min.Industrial, use 70 ℃ first stretching and 100 ℃ second stretching in the stretching-relaxation method usually.Industrial, in the heat treatment staple fibre method, use 70 ℃ first stretch usually, 100 ℃ second stretch and have 0.95 130 ℃ of lax calenders.
Table II: 1.5,2.25, the stretching scheme of 3.0dpf staple fibre
| Stretch yarn dpf not | 4.0dTex | 3.2dTex | 6.4dTex | 6.8dTex | 9.2dTex | 9.7dTex | |
| The first draw ratio D 2/1 | 2.73 | 2.73 | 2.74 | 2.74 | 2.75 | 2.75 | |
| The second draw ratio D 3/2 | 1.10 | 1.10 | 1.15 | 1.15 | 1.20 | 1.20 | |
| The mechanical stretching ratio | 3.00 | 3.00 | 3.15 | 3.15 | 3.30 | 3.30 | |
| Stretching in crimping machine and drier is lax | High | Low | High | | High | Low | |
| 20％ | 16％ | 18％ | 14％ | 16％ | 12％ | ||
| Final staple fibre product | 1.7dTex | 1.7dTex | 2.5dTex | 2.5dTex | 3.3dTex | 3.0dTex |
4.1
The staple fibre performance
Discussion to tensile property is a hypothesis, and bobbin cradle is stretched in the fracture of 90% tow.The typical intensity that stretches lax PTT staple fibre is generally 2.7-3.0cN/dTex, and elongation is generally between the 80-90%.The intensity of typical industrial stretching heat treatment staple fibre is generally 3.4-3.5cN/dTex, and elongation is generally between the 60-65%.The following intensity elongation profile of equilibrium (Fig. 2) will help the possible range near PTT staple fibre performance.Because the PTT tow is lax fast under curling condition, the PTT staple fibre that therefore prepares high strength, low elongation is very difficult.At R﹠amp; The result of test long filament shows on the D equipment, and fibre strength is up to 4cN/Tex under 45% elongation.In the stretching heat treatment method of height optimization, might prepare the PTT staple fibre that intensity is higher than 3.5cN/Tex.In this effort, will be crucial to the control of the condition of curling.
Embodiment 1: extrude with storage process in control undrawn yarn contraction
The contraction of the not stretch yarn of the PTT UDY that evaluation is spun under very wide different condition at two diverse locations.The test result explanation as shown in Figure 5, is preferably in and stores PTT UDY below 31 ℃ to avoid the excessive contraction greater than 2-3%.The figure shows the shrinking percentage in the water-bath of several different temperatures that stretch yarn not immerses 30 ℃, 31 ℃, 32 ℃ and 35 ℃.Spinning condition comprises, for the staple fibre production line of difference exploitation, one at position A, and another is at position B, a series of drawn products dawn number/long filament in 0.8 to the 4.5dpf scope, and the opereating specification of throughput and winding speed.This figure has represented that also PTT UDY shrinkage factor is subjected to the ratio that influences of spinning condition to be subjected to the quench air Temperature Influence bigger.Position A has used 25 ℃ quench air, and position B has used 16 ℃ quench air.
Because if suitably do not control, will increase the variability of staple fibre product, therefore excessive not stretch yarn shrinkage factor is undesirable.
Embodiment 2: staple fibre is handled the contraction of the ptt fiber bar that stretches
Summary and summary:
At 60 ℃ or be higher than any influence that stretches in 60 ℃ the bath and will eliminate that spinning causes to the structure of shrinking with drawing of fiber.
The drawing of fiber shrinkage factor reduces along with the increase of stretch bath temperature, but in temperature during greater than 60 ℃, this influence is very little.Shrinkage factor also reduces along with the increase of total degree of orientation (draw ratio), but this influence is very small under higher stretch bath temperature.When the stretching shrinkage factor was insensitive to spinning and stretching condition, curling became more stable, and product variations is littler.Suggestion stretches being higher than under 60 ℃, and stretches under this condition and will have stable crimp operation.
Drawn from the shrinkage factor data, as the predetermined curling and dry/lax coefficient of relaxation of drier/lax temperature funtion.As if although the shape of this curve is correct, and can be used in the extrapolation of given data, coefficient value is too high.
Product shrinkage factor as drier/lax temperature funtion can infer that this point is seemingly impossible by PTT shrinkage factor data.
Introduce
The spinning condition scope that tests out on this used test draw line is as follows:
● 240-260 ℃ chunk (block) temperature
● 0.432-0.865g/ hole min (0.4mm capillary)
● the spinning speed of 1000-2000m/min
These goods are stretched under three draw ratios:
● stretch ratio at break (BODR)-0.1
●BODR-0.2
●BODR-0.4
A large amount of variations in this and the spun orientation combine, and obtain large-scale spun orientation.
Three staple fibre stretch bath temperature are as follows:
●40℃
●55℃
●70℃
This is the maximum practical operation scope of this equipment.
Stretch fiber strip is characterized comprehensively.To being analyzed as follows of shrinkage factor.
With intensity in PTT, PET and other melt spinning polymer with to stretch mainly be that the function of total degree of orientation is different, contraction is a probe of complicated fibre structure more, and is subjected to the degree of orientation, the more important thing is the influence that is subjected to degree of crystallinity.
The purpose of this part test is to answer following relevant problem of shrinking, and these problems are to provide according to the order to the importance of method design.
Has 1. the difference of spun yarn structure run through whole drawing process? has or drawing process eliminated the difference of spun yarn structure? this has important hint effect for design spinning process and process.
Is 2. the stretch bath temperature how to influence contraction? residual contraction after the stretching is to influence the principal element that how can easily carry out fiber crimp.Usually, the fiber with high shrinkage curls easily.If shrinkage factor is the majorant of the stretch bath temperature and the degree of orientation, crimping machine must be continually by balance is with the variation of reflection stretching condition again, it is inhomogeneous therefore to curl.
Was 3. when fiber stretched and be curling, how many shrinkage factors? and shrinkage factor is influenced by spinning and stretching condition how? coefficient of relaxation is useful to this information in the spinning model for calculating.
4. when relaxing in the baking oven of fiber in uniform temperature, under higher temperature, also have how many extra products to shrink?
Verified have following precursor condition to the useful model of PET:
When being heated to above glass transition temperature, remove unrestrictedly, fiber will shrink the disorientation that becomes up to all amorphous regions.
When temperature is elevated to when being higher than glass transition temperature, other amorphous orientation district occurs along with the fusion of crystal.The amorphous region disorientation of these new generations has produced extra contraction then.Therefore, typical temperature is high more, shrinks big more.
Need several more or less definition of circulation in itself now.Glass transition temperature is defined as, according to thermodynamic (al) second law, and the temperature of the free disorientation of unrestriced amorphous chain.The amorphous region is those zones that do not have crystallization.Crystal region is those zones that do not have disorientation under this temperature.At aspects such as TGA curve, X ray behavior, density, the method for various definitions crystal region is arranged, the method for these definition is more or less different to the answer of degree of crystallinity %, but is correlated with.For the purpose of this discussion, we define crystal according to the ability that they keep being orientated under this temperature.
The essence of this model is hypothesis, and heat treatment one rope only causes crystal fusion and fiber disorientation.For PET yarn lax under the short time of staying, this model is fine.For the staple fibre method of a few minutes time of staying, this model is fairly good, but its validity to PTT is ignorant before this.
Length among Fig. 6, orientation maps will be used to illustrate this method.The figure shows, when being stretched to the sample fiber length l from the length of fiber during at zero birefraction
fThe situation of Shi Fasheng.When this fiber is heated to temperature T
1The time, because all amorphous region disorientation and all are for T
1Unsettled crystal fusion and disorientation, so fiber loss length is to l
1
This fiber is owing to also exist in T
1Therefore stable crystal does not have complete disorientation down.When temperature is elevated to T
2The time, other crystal fusion, become amorphous, disorientation, so length further reduces.Can think, the draw ratio 1.0 in the time of can being retracted to zero birefraction fully, but in fact, when being arranged at fusing point with above fusing point, still stablize in some crystal (this causes the problem in the PET polymerization).These crystal do not have disorientation, so reorientation can not finish forever.
In view of above-mentioned introduction, now, test problem can have been explained.
Does the difference of spun yarn structure run through whole drawing process?
We may expect that shrinkage factor is the majorant of draw ratio, because this provides the reason of the orientation of loss.For PET, this point is more or less correct, and still this influence has seriously been covered by the following fact, and promptly along with the increase of the degree of orientation, the ability that forms the crystalline region has also increased, and therefore orientation being increased has negative effect.Also have in PET, with regard to contraction, under higher stretch bath temperature, all memories of spinning disappear.The degree of orientation can approximate total orientation parameter (TOP) (dawn is counted draw ratio/natural draw ratio) greatly.
In order to calculate natural draw ratio, be necessary to be identified for the suitable strain rate of laboratory equipment and the technology that obtains repeatable result.Under the 200-800%/min strain rate, test is at 40#/hr, the single tube that is spun under 240 ℃ and the 1500m/min.Carry out three retests with being drawn in a curve on the figure.The result has repeatability very much under all strain rates, and good experimental technique and equipment have been described.All decisions have provided the indicatrix that is illustrated among Fig. 3.Natural draw ratio can easily be calculated by these following equatioies:
NDR＝1+(S
n/100) (1)
Wherein, S
nIt is the % strain under the nature elongation strain.
This equals the traditional definition of NDR, and it is defined as:
NDR＝l
d/l
s (2)
Wherein, l
dBe length at the natural drawing point of flexion
l
sBe the length of the sample that is spun into.
The first step is definite, and which variable is important on to statistics during prediction is shunk under the fixed temperature.Its method is in σ statistics (Sigma Stat) 2.0, and in F＞4.0 (F to enter＞4.0), P refusal＜0.05 (P to reject＜0.05) utilizes down progressively forward and homing method backward progressively.
The result who is summarized in the Table III shows:
● in general two kinds of methods are satisfied.
● under 60 ℃ or higher draft temperature, the spinning variable does not play an important role in drawing of fiber shrinks.
● under 45 ℃ of draft temperatures, total orientation parameter and, wonderful chunk temperature is a not too important coefficient in shrinking.
Generally speaking, should utilize 60 ℃ or higher draft temperature to get rid of any spinning influence to the product shrinkage factor.These data have been supported hypothesis, and are promptly the same with PET, if draft temperature apparently higher than Tg, will be got rid of the spinning structure.Utilize r
2＞0.5 regression equation of proofreading and correct is published in the following table.It should be noted that any is,, do not have this regression equation for T＞=60 ℃.
The regression analysis that the Table III ribbon shrinks
| Stretch bath temperature ℃ | Shrink | To Pretesting | Test backward | ||
| Variable | r 2 | Variable | r 2 | ||
| 45 | Boiling | top，T b | 0.666 | top，T b | 0.666 (1) |
| ″ | 125℃ | top，T b | 0.695 | top，T b | 0.695 (2) |
| ″ | 140℃ | top，T b | 0.540 | top，T b | 0.540 (3) |
| ″ | 175℃ | top，T b | 0.489 | top，T b | 0.441 |
| ″ | 197℃ | top | 0.126 | top | 0.126 |
| 60 | Boiling | Q h | 0.190 | Q h | 0.153 |
| ″ | 125℃ | top | 0.188 | Q h | 0.131 |
| ″ | 140℃ | top | 0.241 | top | 0.241 |
| ″ | 175℃ | AVE | na | AVE | na |
| ″ | 197℃ | AVE | na | AVE | na |
| 75 | Boiling | AVE | na | AVE | na |
| ″ | 125℃ | Q h，S m | 0.273 | Q h，S m | 0.273 |
| ″ | 140℃ | AVE | na | AVE | na |
| ″ | 175℃ | AVE | na | AVE | na |
| ″ | 197℃ | AVE | na | AVE | na |
The total orientation parameter of TOP==(dawn is counted draw ratio/natural draw ratio)
T
b=chunk temperature, ℃
Q
h=hole throughput, g/ hole min
S
m=spinning speed, m/min
The independent variable of all eliminatings of AVE=
Is the stretch bath temperature how to influence shrinkage factor? Fig. 7-the 11st is for the figure of the dry-hot shrinkage under the boiling water shrinkage of three used stretch bath temperature and 125 ℃, 140 ℃, 175 ℃ and 197 ℃.Can know and find out that between 45 ℃-60 ℃, the higher temperature of next test has big mechanism and change, and is higher than 60 ℃ in temperature, shrinkage factor almost is independent of the degree of orientation, and responsive relatively to bathing temperature.
Higher bath temperature has reduced potential shrinkage factor on a small quantity, but not remarkable for latent crimp or possible properties of product.
Because the crimping machine operation is very simple, therefore 60 ℃ or higher operating temperature are used in suggestion.Dawn number density (dawn number/linear crimping machine inch, the linear crimping machine cm of dtex/) except enter crimping machine for compensation does not need to adjust crimping machine under these conditions.
Are spinning temperature and stretch bath temperature how to influence coefficient of relaxation? the analysis showed that of Fig. 7-11 and variable, except 45 ℃ of minimum probe temperatures, the potential shrinkage factor of stretching rope is independent of spinning condition, only depends on the degree of orientation slightly.
Figure 12 shows, is used to the stretch oven temperature of rope and the relation between the coefficient of relaxation.Be higher than under 60 ℃ the stretch bath temperature, the straight line by the top group of data points approaches coefficient of relaxation.This is a good starting point, but its value too high (shrinkage factor is too low), and this is because contraction method has used small amount of sample, so it does not freely relax as ground in common factory's drier/lax machine fully.
Yet this curve should have correct shape, and is therefore, when having obtained more mechanical particular data, good to being enough to the Temperature Influence of extrapolating.
Can lax product shrinkage factor be by ribbon shrinkage factor data-speculative?
Can find with the simple contracting model that is used for PET with reference to figure 3, if will be at l
fUnder fiber to put into temperature be T
1Baking oven in, it will lose amorphous orientation, and some crystal are fusion and disorientation, its length will be reduced to l
1Equally, be l with length
fSample to put into temperature be T
2Baking oven in, T wherein
2Be higher than T
1, it will that fusion is shunk under high temperature more be more owing to more crystalline material, and is retracted to length l
2
Arithmetically, shrinkage factor can be represented with following mode:
Suppose: φ
1=T
1Shrinkage factor %/100 (1)
φ
2=T
2Shrinkage factor %/100 (2)
Then, by the definition of xeothermic contraction:
φ
1＝(l
f-l
1)/l
f＝1-l
1/l
f (3)
φ
2＝1-l
2/l
f (4)
If tested at T
1The following sample that has freely relaxed is so at T
2Under what kind of contraction can take place? if in first contraction process, there are not crystal growth or variation rather than fusion and disorientation, it can be retracted to l
2
First contraction is the contraction that fiber carries out in lax machine, and second contraction is the residual shrinkage in lax product.On some degree, PET meets these hypothesis, therefore, can be estimated the shrinkage factor of the product that relaxes by the xeothermic contraction of stretch fiber strip.
For this reason, must calculatively be, at T
1The product of following contraction is at T
2Under the shrinkage factor second time.This can be performed as follows according to definition and Fig. 3 of shrinkage factor:
φ
Ps=(when at T
2Under when shrinking, at T
1The shrinkage factor % of the sample of following contraction)/100 (5)
φ
ps＝(l
1-l
2)/l
1＝1-l
2/l
1 (6)
If equation 3 and 4 is used to eliminate l
1And l
2, the dry-hot shrinkage according to testing under two different temperatures will cause so:
φ
ps＝1-(1-φ
2)/(1-φ
1) (7)
Thus, and the shrinkage factor of test, can calculate at T
1After following baking oven is lax, at T
2Under the desired product shrinkage factor.
Figure 13 is for high-orientation and high the bath under the warm technical useful situation, the figure of prediction shrinkage factor.It shows that after given baking oven was lax, predetermined filament contraction rate was very low.Significant crystal except having taken place the simple disorientation in drier/lax machine, has also taken place and has changed in this explanation.
Embodiment 3: under the strained condition of heating to the evaluation of PTT staple fibre heat setting performance:
The yarn of estimating comprises PTT, PTT/PET mixture, the cotton mixture of PTT/ and PET (Table IV)
In extruding PTT synthetic fiber process, the fracture of long filament will limit production efficiency and product quality greatly.The PTT resin of IV in the 0.55-1.0 scope is preferred, more preferably the resin of IV in the 0.675-0.92 scope, the most preferably resin of IV in the 0.72-0.82 scope.The preparation inherent viscosity is that the PTT synthetic fiber in the 0.72-0.82 scope will significantly not reduce under the prerequisite of final fibre property, helps to improve operability and the product quality that synthetic fiber are produced.
The reduction of PTT inherent viscosity helps:
1. compare with the viscosity of extruding fiber, reduce the variable quantity of section medium viscosity.
2. the uniformity of polymer melt in the improvement filament spinning component.IV is that 0.92 PTT resin requires the production rate limit of strict more filament spinning component filtration system in keeping extruding.
3. improve production operation by the quantity that reduces broken filament in the preparation process.
4. for the long filament of extruding less than 2 dawn/threads, allow to come preparing product with lower extrusion temperature.Known already, PTT degrades being higher than 260 ℃ melt extrude under the temperature.When to utilize IV be 0.92 thin dawn synthetic fiber of resins (less than the long filament of 2dpf), must increase and melt extrude temperature and melt viscosity is enough to be reduced to avoids excessive melt turbulent flow and melt degraded, these all cause the filament breakage in the extrusion.
5. reduce the amount of contraction in the product fiber, make it easier and carry out stretched operation and/or be wound into stable yarn packages.
The short fiber yarn of being made by PTT has the recoverable elasticity of wonderful elasticity-have when extending to the 15-25% of yarn original length.This elasticity also is present in by in the short fiber yarn that closely and not the tight fibers mixture is made, and wherein PTT is the main fibre fractionation with weight and/or length gauge.In addition, this elasticity is recoverable after hundreds of changes.This elasticity is enough to improve the shape retention properties by PTT short fiber yarn and the thread textiles of mixing short fibre yarn.Suitably construct and arrangement contains the fabric of most of PTT short fiber yarns (with the weight percent meter of length), can in woven and knit goods, have wonderful high elasticity restorative (manual 500 circulations and instrument 200 circulate more than test).The present invention has covered and has changed staple fibre the yarn texture of twisting into by any method and make spun staple yam.This spun yarn can be made the equipment that staple fibre becomes yarn by craft, charkas, ring spinning, open-end-spinning, air-jet spinning or other type.
The short fiber yarn of being made by cotton, hair, acrylic compounds, PET does not have elasticity.In order to make resilient short fiber yarn by these fibers, industrial having to usually in inside added a kind of elasticity continuous filament yarn in yarn or in fabric, make final fabric product have elasticity.These schemes are more expensive than the basic spun staple yam of being made by PTT.Value of the present invention is, people can utilize basic spun staple yam technology preparation that the elasticity spun yarn of industrial value is arranged, and do not need to invest more expensive bag core spun yarn equipment or in fabric construction, sneak into the elasticity continuous filament yarn, the latter will make coloration of textile materials and put in order complicated.
Attempt characterizing simply, staple fibre heat setting performance is how to influence by the PTT staple fibre and be mixed with cotton PTT staple fibre and the performance of the yarn that the PTT staple fibre that mixes with the PET staple fibre is made.As shown in Table IV, PET and cotton mixed yarn by several PTT staple fibre supplier in different lax machine temperature with have under visibly different the curling and make.Therefore, can not determine realizingly with the immixture of other fiber.Therefore, should cautiously test the accurate mixing ratio of deriving by these.This test is will look in each embodiment yarn about amount of contraction, modulus, stress decay and restorative several aspect.These factors normally independently, and in this work separately research.
Table IV: fibre property
| Project | PTT5-CR1-2 | PTT5-CR1-3 | PTT-CR1-4 |
| The lax oven temperature of fiber ℃ | 105 | 120 | 135 |
| Fiber Denier/threads | 1.75 | 1.80 | 1.79 |
| Intensity, cN/dtex | 3.52 | 3.49 | 3.24 |
| Extension at break, % | 48 | 45 | 44 |
| Load under 10% strain, cN/dtex | 0.83 | 1.21 | 1.13 |
| Manual crimp index, % | 28 | 19 | 18.5 |
| Curl/inch | 14.8 | 15.8 | 14.2 |
| The yarn of making | 100 | 50%PTT and 50 | 50%PTT and 50%PET |
General introduction and summary
For the dry-hot shrinkage under 175 ℃ on the spun yarn
● for the mixture (100%PTT, 100%PET, 50/50 PTT/PET and 50/50 PTT/ cotton) of all tests, the spun yarn dry-hot shrinkage reduces along with oven temperature.
● for the mixture of all tests, for per 1% apply elongation (or lax), xeothermic contraction approximately increases by 1/2%.
● the little 2-2.5% of PTT spun yarn shrinkage ratio PET yarn.
● the PTT data tightly servo-actuated in the amorphous disorientation model that is used to shrink.
The boiling water shrinkage of spun yarn
● for the mixture of all tests, boiling water shrinkage reduces along with oven temperature.
● for the mixture of all tests, for per 1% the elongation that applies, boiling water shrinkage increases about 0.4%.
● owing to the PTT spun yarn is prepared by the stretching relaxation method, and the PET sample is prepared by the stretching heat treatment method, so the PTT spun yarn approximately hangs down 1% than the boiling water shrinkage of PET yarn.
The load of spun yarn under 5% strain (elongation)
When the very little power of needs caused the length significant change, this fabric was considered to " resilient ".In this group test, we select fabric generation strain 5% needed power to characterize elongation.The primary variables that influences the mixture of all tests is the elongation that applies.Oven temperature is not very important, and this evaluation shows:
● PTT is low 3-4 times at the force rate PET that elongation 5% o'clock (bigger elongation) needs.
● the PTT elongation is along with the decrease of the elongation that applies is 1/10 (0.01gpd increases by/1% elongation to the 0.1gpd/1% elongation) of PET.Therefore, can apply elongation to the PTT employing and not have big yarn elongation loss to change yarn property.
● the elongation of 100%PTT yarn is quite insensitive concerning heat-setting condition.
The spun yarn stress decay
A kind of yarn or fabric will recover how much to depend on two factors after certain time under certain strain:
1. how many stress decaies is when keeping strain.
2. how many amounts of recovery after the release strain is.
These factors usually normally independently, and in this work separately research.
● the PTT stress decay is independent of heat-set temperature, and the linear reduction along with the increase of the elongation that applies (whenever applying 1% elongation in stress decay reduction by 0.5%/heat setting)
● the PET stress decay reduces along with the increase of oven temperature, and the linear reduction along with the increase of the elongation that applies.The elongation effect that applies is considered to bigger (0.9%/1% elongation that applies) than PTT.
● PTT and PET have the stress decay of substantially the same amount.
● the behavior of PTT/PET blended yarns is positioned at the centre of corresponding pure yarn, has-0.7% reduction/apply 1% elongation.
● the cotton blended yarns stress decay of PTT/ is independent of heat-setting condition.
Spun yarn is restorative
Restorative (98% restorative) of restorative pre-industry (pre-commercial) yarn samples well below nearest test of the PTT yarn that obtains by this group sample.Its reason may be to have used 100 ℃ drier baking oven in fiber treatment.Influencing the restorative main heat setting variable of all specimen is the elongation that applies, along with the restorative increase of the increase of the elongation that applies:
● the restorative increase by 0.9% of PTT/apply 1% elongation.
● PTT is usually than the restorative high 5-10% of PET.
● the data of the cotton mixture of PTT/ are very unstable, but have the general trend identical with pure yarn.
Shrink basic principle
In containing the semi-crystalline polymer fiber of a large amount of orientations, orientation is present in two zones, crystal region and the amorphous region that is connected with crystal region.Usually the crystalline size that has certain limit, the orientation of crystal region also may change.
Be lower than glass transition temperature when following when fiber is placed, length variations is very slow, and is called creep.Usually, useful textile fabric is not having under the load, and creep rate is all very low.When fiber was heated to above glass transition temperature, the amorphous region activity that becomes, and under power without limits was as much as possible near isotropic state disorientation (not having preferred orientation).The isotropic state is supported by second law of thermodynamics.This causes contraction usually, but under a few cases, crystal region self collapse, and " bearing " orientation is arranged, so fiber increases.This fiber is called that self is tensile.But do not know whether they can be made by PTT.Crystal region is inactive, and also disorientation not.
Along with the continuation increase of fiber temperature, less crystal fusion, and their zone becomes amorphous.At this moment, their disorientation and extra contraction takes place.Here it is for semi-crystalline polymer, the reason why shrinkage factor raises along with temperature usually.Therefore, there are two kinds of strategies that reduce the filament contraction rate:
1. wishing contraction in advance under the stable temperature of fiber.
2. under producing under the temperature of stable crystal to the temperature of not wishing filament contraction, crystallization under heat and tension force.
For commodity PET fiber, this moment, problem was spinning and woven efficient and yarn strength, and the second route is extremely useful, because we can see subsequently, and the pre-modulus that has reduced fiber of shrinking.Special fibre particularly for the wool mixture, uses article one route, because intensity and modulus no longer are important problem, but the better dyeability that route 1 provides is favourable.On this abutment, which bar route is better for PTT, is unclear.
Extended as fruit fiber, its amorphous orientation increases, so shrinkage factor increases.In the non-twist continuous filament yarn yarn of PET, normally near 1 pair 1 (promptly increase by 5% elongation, just increase by 5% shrinkage factor).
Up to now, we have discussed not crimped fibre of list.Will be complicated more for the situation of spun yarn, this be because:
● fiber is twisted on spiral angle, and this has reduced the contraction of fiber in the yarn.
● in the middle of fiber is moved to from the outside of yarn.
● fiber may slide in yarn.
● can change the shrinkage factor of assembly with the existence of the blended fiber of different shrinkage factors.
Even have these complexity, we still can utilize this naive model to predict the response of spun yarn to heat-setting condition:
1. if with yarn heating and make it freely to relax, it also will increase disorientation and degree of crystallinity.These two factors have all reduced shrinkage factor.Under constant oven temperature, the reduction of shrinkage factor will be with lax linear.Shrinkage factor will reduce along with the increase of oven temperature.
2. if with yarn heating and maintenance constant length, do not have disorientation.As long as the yarn treatment temperature of oven be higher than fiber make in the temperature of fiber in the free relaxation step process, shrinkage factor will reduce along with the increase of oven temperature.
3. if yarn is heated and is extended, orientation increases, so shrinkage factor increases.Shrinkage factor will linearity increase along with the elongation that applies, and reduce along with the increase of oven temperature, and prerequisite is that oven temperature is higher than the temperature in the fiber treatment process.
Given this, just analyze the influence of heat-setting condition now easily to the yarn shrinkage factor.
175 ℃ of xeothermic contractions of spun yarn
As shown in figure 14, PTT is a fabulous matrix of observing total orientation model strictly all rules.
Applying for 0% when elongation, 100 ℃ of lax down comparisons almost have with 100 ℃ of identical contractions of yarn of processing down.When handling under higher temperature, still under constant length, shrinkage factor reduces.
Because length is to change by elongation or the shrinkage factor that applies, so shrinkage factor increases along with the elongation that applies is linear, and its slope is along with the variation of oven temperature is almost constant.Under 176 ℃ given oven temperature, xeothermic being punctured into whenever applies 1% elongation and increases about 0.46%.
As shown in figure 15, the behavior of PET and PTT's is similar.Because it is heat treatment of fibre, rather than relaxed fibre, even therefore under 100 ℃, the shrinkage factor of contrast yarn also reduces along with the increase of oven temperature.Because it has high-modulus, therefore in the height elongation with hang down under the oven temperature, fiber does not extend yet, but fiber slides in the yarn, so the increase of shrinkage factor does not have, and PTT's is big like that.For the oven temperature that is higher than 130 ℃, the dry-hot shrinkage of PET is whenever to apply 1% approximately increase by 0.55% of elongation.This is more or less higher than PTT's, but both are commented experience estimation, and approximately per 1% elongation increases by 0.5% shrinkage factor.
Figure 16 has compared PTT and the shrinkage factor of PET yarn under the highest and minimum heat-set temperature.Under identical oven conditions, the dry-hot shrinkage of PTT is approximately than the low 2-2.5% of PET.As mentioned above, the two shrinkage factor increases much at one along with the elongation that applies.
The shrinkage factor of the cotton mixture of PTT/ increases along with the increase of the reduction of oven temperature and the elongation that applies, similar (Figure 17) of this point and PET mixture.It increases along with the elongation that applies is almost linear, whenever applies 1% elongation, and shrinkage factor approximately increases by 0.47%.For conditions of similarity, about low 1% of the shrinkage ratio PET mixture of cotton mixture.For this group sample, comment experience estimation, whenever apply 1% elongation, dry-hot shrinkage increases by 0.5%.
The spun yarn boiling water shrinkage
Except amorphous orientation is to be present in the fiber and at all crystals of fusion between glass transition temperature and 100 ℃, boiling water shrinkage is identical with the dry-hot shrinkage behavior, so it is well below dry-hot shrinkage.In some fiber that wherein plasticization of water is high, this contraction is considerable.The fiber that is higher than 100 ℃ stretching relaxation method preparation by lax temperature has low-down boiling water shrinkage usually.Heat treatment of fibre has high relatively boiling water shrinkage usually, and this is because they are heated under tension force and always have amorphous orientation.
These samples are generally observed these principles.All mixtures show and the behavior together of xeothermic contraction phase, and promptly shrinkage factor reduces along with the increase of oven temperature, increases along with the elongation that applies.
PTT contrast yarn has 2% shrinkage factor, even it is lax down at 100 ℃ to form its fiber.This explanation in process, may be in the carded process, has produced some cold stretch.If the modulus of PTT is low, this also is among expecting.PTT yarn shrinkage factor increases about 0.38% for whenever applying 1% elongation.Contrast PET yarn is owing to by the heat treatment method preparation, therefore have higher shrinkage factor (4.5% pair 2%) relatively than PTT.The yarn shrinkage factor is whenever to apply 1% elongation increase by 0.47%.Suppose yarn heat setting conditional likelihood, in general, the dry-hot shrinkage of PTT yarn is than about low 1% (Figure 18) of PET yarn.
The shrinkage factor of PTT/PET blended yarns is whenever to apply 1% elongation increase by 0.44%, and the PTT/ cotton increases by 0.417%.Comment the experience estimation boiling water shrinkage, for all test conditions, whenever applying 1% elongation increases about 0.4%.
For 100% PTT spun yarn, the load under 5% strain almost is independent of oven temperature, and linear with the elongation that applies, and whenever applies 1% elongation increase 0.01gpd.This explanation, owing to yarn stretches in the heat setting process, so yarn elongation reduces.The PTT data declaration under 5% strain, almost has identical load with yarn in 0 elongation and 100 ℃ of following heat settings by the contrast yarn of making at 100% time lax fiber.
The behavior of PET yarn is similar.At this moment, yarn has sizable change with respect to 100 ℃ of following heat settings with apply the contrast yarn of zero elongation, this be since raw fiber by heat treatment, and not lax.The order of magnitude of load of PET under 5% elongation is higher than the PTT that has applied elongation, and whenever applying 1% elongation is 0.1gpd.
Figure 19 has contrasted the behavior of PTT and PET, and the elongation advantage of PTT is significant.Be not only not apply the low 3 times of elongation for the needed force rate of 5% strain, and also very little to the response that applies elongation, this explanation, can apply elongation and need not with excessive sacrifice yarn elongation in heat setting PTT yarn is cost.Interesting is, the PET sample that has applied the force rate lax 7.5% that the PTT sample (7.5%) of maximum elongation needs when 5% strain is little by 45%.
The spun yarn stress decay
A kind of yarn or fabric are in the generation strain and after continuing for some time under the constant length, and the amount of recovery of strain depends on two factors:
How many stress decaies have taken place when sample remains on constant length following time.Opposite extreme situations is that if all stress has all lost, recovery will be zero.
How many amounts of recovery of strain is after the testing time section.
This spun yarn stress decay test comprises: 5% strain takes place in yarn, then spun yarn is kept 2 minutes under this length, and makes yarn return to zero stress.Manually compute stress decay by resolution chart, this method is more or less more inaccurate than the instrument calculated data that obtains from computer analysis method.Stress decay and restorative be two independently phenomenons, divide the discussion of coming.
The stress decay of 100%PTT yarn is independent of oven temperature, and the linear reduction along with the elongation that applies.Although think that instinctively stress decay should increase along with the elongation that applies, be the r of its correction
2Very high.The stress decay of PTT is whenever to apply 1% approximately reduction by 0.5% of elongation.Although certain oven temperature effect is arranged, the behavior of PET yarn is similar, and the reduction amount (decay 0.9%/apply 1% elongation) that whenever applies 1% elongation is almost the twice of PTT.Figure 20 has compared the stress decay of PTT and PET.In general, PET applies under the elongation higher than PTT low, and at high oven temperature with lowly apply under the elongation lower than PTT.The behavior of PTT/PET mixture is in the middle of two kinds of pure fibers, and is more insensitive to oven temperature, for the stress decay that whenever applies 1% strain reduces by 0.7%.The stress decay of the cotton mixture of PTT/ is independent of heat-setting condition.
Spun yarn is restorative
The restorative influence that is not subjected to oven temperature of PTT, and the linear increase along with the increase of the elongation that applies (whenever applying 1% elongation, restorative increase by 0.9%).The restorative of PET increases more or less along with the increase of oven temperature, but main influence is the elongation that applies.Its response ratio PTT's is more obvious, whenever applies 1% elongation, restorative increase by 2.2%.As shown in figure 21, except PET wherein has the high elongation that applies under high oven temperature, PTT's is restorative usually than the high 5-10% of PET.The response of PTT/PET mixed yarn is identical with pure PTT's, and is irrelevant with oven temperature, and the elongation that applies is had strong response (whenever applying 1% elongation, restorative increase by 1.7%).The cotton mixture of PTT/ some is strange as a result, along with higher oven temperature with bigger apply elongation, restorative increase.
The trade-off of the performance in the spun yarn heat setting
The one of the main reasons of doing this work is to answer: " if the heat setting yarn has reduced its shrinkage factor, so elongation, restorative and stress decay variation what? " in order to answer this problem from these group data, these variablees are necessary to draw.Because all variablees are correlated variabless, therefore only for these group data and wherein correlated variables be and we in other data of this same way as of doing variation, this relation is correct.Given this, let us is observed its reflection:
For the trade-off of elongation/dry-hot shrinkage, elongation increases (load under 5% strain reduces) along with the reduction of dry-hot shrinkage.This is favourable rule, because by allowing yarn shrink the shrinkage factor that reduces, do not lose elongation.Although r
2Very low, be 0.47, consider to comprise each point, so these data may be reliable trend guiding.Load under every reduction by 1%, 5% strain of shrinkage factor reduces 0.01gpd.
The trade-off of restorative/dry-hot shrinkage is disadvantageous.The every reduction by 1% of dry-hot shrinkage, restorative reduction by 1.3%.The r of these data
2Considerable, be 0.64.
The exchange of stress decay/dry-hot shrinkage is disadvantageous, the every increase by 1% of dry-hot shrinkage, and stress decay increases by 0.9%.We think that this increase of stress decay is corresponding to restorative reduction.At any time, dry-hot shrinkage only should be reduced to the needed minimum of a value of user.
Embodiment 4: in PTT staple fibre preparation, the IV of PTT resin is reduced from 0.92
To 0.82, improved and extruded reliability
The fracture of long filament has limited production efficiency and product quality greatly in the PTT synthetic fiber extrusion.The preparation inherent viscosity is that the PTT synthetic fiber in the 0.72-0.82 scope help to improve synthetic fiber production operation and product quality, and does not significantly reduce the performance of final fiber.
The reduction of PTT inherent viscosity helps to reduce the variable quantity of the intrinsic viscosity of comparing with the viscosity of extruding fiber.It has also improved the uniformity of polymer melt in the filament spinning component.IV is that 0.92 PTT resin needs the production rate limit of harsh more filament spinning component filtration system in guaranteeing to extrude.It also improves production operation by the quantity that reduces broken filament in the production process simultaneously.For the long filament of extruding less than 2dpf, allow to use lower extrusion temperature.PTT degrades under the melt extrusion temperature that is higher than more than 260 ℃, and this point is known.When utilizing IV is when thin dawn of resins of 0.92 counting synthetic thread (less than the long filament of 2dpf), we have to increase the melt extrusion temperature and melt viscosity is reduced to is enough to melt turbulent flow and the melt degraded of avoiding too much, and it causes filament breakage in the extrusion.It has also reduced the amount of contraction in the fiber product, makes it the stable yarn bag of easier stretched operation and/or coiled.
Claims (10)
1. one kind is utilized polytrimethylene terephthalate PTT to prepare the method for textile staple on existing PET textile staple production equipment, comprising:
(a) under 245 ℃-253 ℃, melt extrude the PTT polymer,
(b) utilize at least one spinning plate with the PTT spun yarn of extruding,
(c) spun yarn is moved to first take up roll, wherein the distance between this roller and the spinning plate is the 16-20 foot,
(d) spun yarn was cooled to be lower than 31 ℃ before arriving first take up roll,
(e) randomly, spun yarn is stored under the temperature that is not higher than 31 ℃,
(f) before stretched operation, under at least 60 ℃, this yarn of preconditioning under tension force,
(g) at least 60 ℃ of following drawings,
(h) randomly, make drawing down lax up to 190 ℃ and
(i) descend curling drawings at 70 ℃-120 ℃, and the feeding speed of drawing is reduced the 10-60% dawn by the drawing feeding speed for preparing corresponding PET.
2. according to the process of claim 1 wherein that the inherent viscosity of PTT is 0.55-1.0.
3. according to the method for claim 2, wherein the inherent viscosity of PTT is 0.72-0.82.
4. according to the process of claim 1 wherein that spun yarn was cooled to below 25 ℃ before arriving first take up roll.
5. do not use relaxation step according to the process of claim 1 wherein, and curling temperature is 70-100 ℃.
6. according to the process of claim 1 wherein the use relaxation step, and curling temperature is 80-120 ℃.
7. according to each method among the claim 1-6, wherein step (i) also comprises the crimping machine volume that uses than the big 10-50% of crimping machine volume that is used to prepare corresponding PET.
8. according to each method among the claim 1-6, wherein drawing feeding speed reduces 40-60%.
9. one kind is having the method that is prepared textile staple on the PET textile staple production equipment by polytrimethylene terephthalate PTT now, comprising:
(a) under 245 ℃-253 ℃, melt extrude the PTT polymer,
(b) utilize at least one spinning plate with the PTT spun yarn of extruding,
(c) spun yarn is moved to first take up roll, wherein the distance between this roller and the spinning plate is the 16-20 foot,
(d) spun yarn was cooled to be lower than 31 ℃ before arriving first take up roll,
(e) randomly, spun yarn is stored under the temperature that is not higher than 31 ℃,
(f) before stretched operation, under at least 60 ℃, this yarn of preconditioning under tension force,
(g) at least 60 ℃ of following drawings,
(h) randomly, make drawing down lax up to 190 ℃ and
(i), and use crimping machine volume than the big 10-50% of crimping machine volume that is used to prepare corresponding PET at 70 ℃-120 ℃ following curling drawings.
10. according to each method in claim 1-6 and 9, wherein step (g) comprises two-step stretch at least, the first step is to carry out under at least 60 ℃, and second kind and stretching subsequently, if present, be under the temperature of yarn fusing point, to carry out in the temperature higher than first draft temperature.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US18953100P | 2000-03-15 | 2000-03-15 | |
| US60/189,531 | 2000-03-15 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1425082A CN1425082A (en) | 2003-06-18 |
| CN1179074C true CN1179074C (en) | 2004-12-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB018082173A Expired - Fee Related CN1179074C (en) | 2000-03-15 | 2001-03-15 | Poly (trimethylene) terephthalate textile staple production |
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| Country | Link |
|---|---|
| EP (1) | EP1264019B1 (en) |
| JP (1) | JP2003527497A (en) |
| KR (1) | KR100688822B1 (en) |
| CN (1) | CN1179074C (en) |
| AT (1) | ATE298810T1 (en) |
| AU (1) | AU2001247437A1 (en) |
| BR (1) | BR0109290A (en) |
| CA (1) | CA2402533C (en) |
| DE (1) | DE60111724T2 (en) |
| ES (1) | ES2243474T3 (en) |
| MX (1) | MXPA02009026A (en) |
| WO (1) | WO2001068962A2 (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6752945B2 (en) | 2000-09-12 | 2004-06-22 | E. I. Du Pont De Nemours And Company | Process for making poly(trimethylene terephthalate) staple fibers |
| US6458455B1 (en) | 2000-09-12 | 2002-10-01 | E. I. Du Pont De Nemours And Company | Poly(trimethylene terephthalate) tetrachannel cross-section staple fiber |
| US7578957B2 (en) * | 2002-12-30 | 2009-08-25 | E. I. Du Pont De Nemours And Company | Process of making staple fibers |
| EP1479802B1 (en) * | 2003-05-05 | 2016-02-24 | Amann & Söhne GmbH & Co. KG | Sewing thread and process of making such a sewing thread |
| CN1712592B (en) * | 2004-06-22 | 2010-09-29 | 浙江云山纺织印染有限公司 | Spinning process of polybutylene propalid fibre |
| KR100664164B1 (en) * | 2004-10-27 | 2007-01-04 | 엘지전자 주식회사 | Apparatus for controlling angle of folder open/close in mobile phone |
| CN1827873B (en) * | 2006-03-30 | 2010-11-03 | 宜宾丝丽雅股份有限公司 | Composite yarn manufacturing method |
| JP4943771B2 (en) * | 2006-08-21 | 2012-05-30 | 帝人ファイバー株式会社 | Polyester staple fiber |
| CN102138709B (en) * | 2011-05-10 | 2013-03-27 | 丹阳市丹祈鱼跃纺织有限公司 | Method for preparing maize biology-based special-leather-feel top grade leisure shell fabric |
| WO2013074453A2 (en) * | 2011-11-18 | 2013-05-23 | E. I. Du Pont De Nemours And Company | Process for preparing bicomponent fibers comprising poly(trimethylene terephthalate) |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2038039A5 (en) * | 1969-03-12 | 1970-12-31 | Fiber Industries Inc | |
| TW288052B (en) * | 1994-06-30 | 1996-10-11 | Du Pont | |
| AR001862A1 (en) * | 1995-05-08 | 1997-12-10 | Shell Int Research | Spinning of poly (trimethylene terephthalate) in carpet grade yarns |
| JPH11189938A (en) * | 1997-12-24 | 1999-07-13 | Toray Ind Inc | Polypropylene terephthalate staple fiber and its production |
| US6109015A (en) * | 1998-04-09 | 2000-08-29 | Prisma Fibers, Inc. | Process for making poly(trimethylene terephthalate) yarn |
| JP4009370B2 (en) * | 1998-08-24 | 2007-11-14 | ユニチカ株式会社 | Production method of polyester fiber |
| JP2000220067A (en) * | 1999-01-26 | 2000-08-08 | Toray Ind Inc | Polypropylene terephthalate nonwoven fabric |
| DE19934551A1 (en) * | 1999-07-22 | 2001-01-25 | Lurgi Zimmer Ag | Polytrimethyleneterephthalate staple fibers for textile, especially carpet manufacture, have specific properties and can be dyed with dispersion colors without addition of a carrier |
-
2001
- 2001-03-15 WO PCT/US2001/008230 patent/WO2001068962A2/en active IP Right Grant
- 2001-03-15 BR BR0109290-1A patent/BR0109290A/en not_active Application Discontinuation
- 2001-03-15 JP JP2001567836A patent/JP2003527497A/en active Pending
- 2001-03-15 DE DE60111724T patent/DE60111724T2/en not_active Expired - Fee Related
- 2001-03-15 ES ES01920379T patent/ES2243474T3/en not_active Expired - Lifetime
- 2001-03-15 EP EP01920379A patent/EP1264019B1/en not_active Expired - Lifetime
- 2001-03-15 AU AU2001247437A patent/AU2001247437A1/en not_active Abandoned
- 2001-03-15 CA CA2402533A patent/CA2402533C/en not_active Expired - Fee Related
- 2001-03-15 MX MXPA02009026A patent/MXPA02009026A/en active IP Right Grant
- 2001-03-15 KR KR1020027012125A patent/KR100688822B1/en not_active IP Right Cessation
- 2001-03-15 AT AT01920379T patent/ATE298810T1/en not_active IP Right Cessation
- 2001-03-15 CN CNB018082173A patent/CN1179074C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| KR100688822B1 (en) | 2007-02-28 |
| CN1425082A (en) | 2003-06-18 |
| CA2402533A1 (en) | 2001-09-20 |
| PL357910A1 (en) | 2004-08-09 |
| BR0109290A (en) | 2002-12-17 |
| WO2001068962A3 (en) | 2002-01-31 |
| WO2001068962A2 (en) | 2001-09-20 |
| CA2402533C (en) | 2010-04-27 |
| ES2243474T3 (en) | 2005-12-01 |
| DE60111724D1 (en) | 2005-08-04 |
| MXPA02009026A (en) | 2003-04-25 |
| DE60111724T2 (en) | 2006-05-04 |
| EP1264019B1 (en) | 2005-06-29 |
| KR20020091131A (en) | 2002-12-05 |
| AU2001247437A1 (en) | 2001-09-24 |
| EP1264019A2 (en) | 2002-12-11 |
| ATE298810T1 (en) | 2005-07-15 |
| JP2003527497A (en) | 2003-09-16 |
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