EP1330563B1 - Method for the spinning and winding of polyester filaments, polyester filaments obtained by the spinning method, draw texturing of the polyester filaments and bulked polyester filaments obtained by draw texturing - Google Patents

Abstract

Production of preoriented and melt spun polyester filaments comprising 90 wt.% of polybutylene terephthalate (PBT) of the total polyester filament weight and/or polytrimethylene terephthalate (PTMT) involves setting the spin draft, cooling directly and bundling together at a gap of 500-2500 mm. Production and winding of preoriented and melt spun polyester filaments comprising at least 90 wt.% of polybutylene terephthalate (PBT) of the total polyester filament weight and/or polytrimethylene terephthalate (PTMT) and is preferably wholly of PTMT. The spin draft is set at 70-500. The filaments are cooled directly on leaving the spinneret for a length of 30-200 mm, to a temperature below the setting point, and bundled together at a gap of 500-2500 mm from the under side of the spinneret. The filament tension before and between the godet rollers is 0.05-0.20 cN/dtex. The filament winding speed is 2200-6000 m/min. The polyester contains a polymer additive to increase its stretch, mixed in at a rate of 0.05-2.5 wt.% of the total filament weight. Independent claims are included for: (1) preoriented polyester filaments which, after four weeks of storage, have a stretch to break of 90-165%, a boiling shrinkage of at least 30%, a normal uster of =1.1%, a double refraction of 0.030-0.058, a density of =1.35 g/cm 3> and preferably =1.33 g/cm 3>, a variation coefficient of the shearing load and stretch to break of =4.5%; and (2) a bulked polyester filament, where the POY yarns are passed through a draw texturizing unit at a speed of at least 500 m/min. with a drafting ratio of at least 1:1.35 to give a bulked filament yarn with a shear strength of >=26 cN/tex and a stretch to break of >=30% or >=36%.

Description

The present invention relates to methods for spinning and winding of Preoriented polyester filaments, which are based on at least 90 wt .-% the total weight of the polybutylene terephthalate (PBT) polyester filament and / or polytrimethylene terephthalate (PTMT), preferably from PTMT, and the preoriented polyester filaments obtainable by the process. Furthermore, the present invention also relates to Process for stretch texturing the spun and wound polyester filaments and the bulky ones obtainable by stretch texturing Polyester filaments.

The production of continuous polyester filaments, in particular of Polyethylene terephthalate (PET) filaments, in a two-stage process already known. In the first stage, smooth preoriented filaments are produced spun and wound, the finished in a second stage and stretched heat-set or stretch-texturized to bulky filaments.

An overview of this is provided by the book Synthetic Fibers by F. Fourné (1995), published by Hanser-Verlag Munich. However, only the Production of PET fibers described, with no closed Rather, an overview is presented in which the various features are described.

The fiber production of various spinnable polymers, among others Polypropylene, polyamides, polyesters, etc. are the subject of the application DE-OS 38 19 913. However, in the examples only the production of PET-Fasem described how this can be taken from the temperature at which the Polymer is processed.

In the preparation of continuous polytrimethylene terephthalate (PTMT) -or Polybutylene terephthalate (PBT) filaments has the problem that Preoriented filaments both directly after spinning and when winding as even several hours after rewinding when storing in Ambient temperature have a considerable tendency to shrink, resulting in a Thread shortening leads. The bobbin is thereby compressed, so that it in extreme cases, a shrinkage of the bobbin on the Aufspuldom comes and the winding body can not be removed. Farther forms in the winding body, a so-called saddle with hard edges and run in middle part. As a result, textile characteristics of the filaments, such as the Uster more uneven and there are flow problems when working off the wraps. Remedy then only the restriction of the Coiling weight to less than 4 kg. Such problems occur in the Processing of PET fibers does not occur.

Furthermore, it is observed that, in contrast to PET filaments, preoriented PBT or PTMT filaments reinforced during storage. It occurs one Structure hardening, which leads to such a strong drop in the Cooking shrinkage leads that a Nachkristallisation can be detected. Such PBT or PTMT filaments are for further processing only conditionally suitable, they lead to errors in the stretch texturing and to a Significant reduction in tear strength of the textured yarn. The Lowering the texturing speed or the draw ratio is the episode.

These differences between PET and PBT or PTMT are due to structural and Attribute differences, such as those in Chemical Fibers Int., P. 53, vol. 50 (2000) and theme on the 39th Int. Man made Fiber Congress, from 13 to 15 Sept. in Dombim. So will assume that different chain formations for the Property differences are responsible.

First approaches to solving these problems are described in the patent application WO 99/27168 and European Patent EP 0,731,196 B1. WHERE 99/27168 discloses a polyester fiber comprising at least 90% by weight Polytrimethylene terephthalate and a boiling shrinkage between 5% and 16% and an elongation at break of 20% to 60%. The production of in WO 99/27168 described polyester fiber is made by spinning and Stretching. This spin spinning speeds of at most 2100 m / min specified. The procedure is due to the low Spinning speed uneconomical. In addition, the obtained Polyester fibers, as the indicated figures show, strongly crystalline and thus only partially suitable for draw texturing.

European patent EP 0,731,196 B1 claims a method for spinning, Stretching and winding a synthetic thread, with the thread after the stretching and before winding to reduce the Shrinkage is subjected to a heat treatment. usable Synthetic fibers also include polytrimethylene terephthalate fibers. According to EP 0,731,196 B1, the heat treatment is carried out in that the synthetic Thread in close proximity but substantially without contact along an elongated heating surface is performed. The application of a Heat treatment makes the process more expensive and also supplies synthetic threads with high crystallinity, which are only partially suitable for draw texturing.

In the article by Dr. H.S. Brown and H.H. Chuah; "Texturing of textile filament yarns based on polytrimethylene terephthalate "Chemical Fibers International, Volume 47, Feb. 1997, pp. 72-74, the draw texturing of pre-oriented polytrimethylene terephthalate filaments Texturing speeds of 450 m / min and 850 m / min described. According to this disclosure is the lower texturing speed of 450 m / min for Polytrimethylene terephthalate filaments more suitable, since in this case fibers obtained with better material properties. The tensile strength of the Polytrimethylene terephthalate fibers is 26.5 cN / tex (Texturing speed of 450 m / min) or 29.15 cN / tex (Texturing speed of 850 m / min) and the elongation at break of 38.0% (Texturing speed of 450 m / min) or 33.5% (Texturing speed of 850 m / min) specified.

The document WO 01/04393 describes PTMT filaments which have a Boiling shrinkage in the range of 3 to 40%. This value will however determined immediately after the production of the filaments. After a storage period of 4 weeks under normal conditions, this value decreases below 20% as this the attached Figure 1 shows.

Figure 1 describes the change in boiling shrinkage for three PTMT-POY coils depending on the storage time under normal climatic conditions. in this connection was the change in the POY cooking shrinkage for three coils with different initial value over the storage time at normal Climatic conditions examined. The spools No. 16 and 17 with high Initial value> 40% show after 4 weeks a boiling shrinkage above 30%, preferably above 40%. If the initial value of the boiling shrinkage However, less than 40%, so the coil 18 shows that this after 4 weeks Storage time, however, falls below the critical value of 30%.

FIG. 2 schematically shows force-strain diagrams of PTMT-POY same elongation at break, Figure 2a) shows a diagram according to the invention a natural draw ratio (NVV) equal to or greater than 15%, and Figure 2b) is a diagram with NVV = 0%.

The shrinkage is a measure of the processability and the Degree of crystallization of the fibers. The fibers described in WO 01/04393 have Plastics with a higher degree of crystallization, which is essential worse and only at lower draw ratio and / or lower Process the texturing speed.

In view of the prior art, it has now been the object of the present invention to provide a method for spinning and winding pre-oriented polyester filaments consisting of at least 90% by weight, based on the total weight of the PBT and / or PTMT filaments to provide, which allows the production and winding of pre-oriented polyester filaments in a simple manner. In particular, the polyester preoriented filaments should have elongation at break values in the range of 90% -165%, a high uniformity in filament characteristics and a low degree of crystallinity.
Another object of the present invention was to provide a method for spinning and winding of pre-oriented polyester filaments, which is industrially and inexpensively feasible. The method according to the invention should allow as high take-off speeds, preferably greater than 2200 m / min and high thread weights on the bobbin of more than 4 kg.

It was also an object of the present invention to improve the shelf life of the invention Preoriented polyester filaments obtainable by the process according to the invention to improve. These should also be for a longer period, for example, 4 weeks, be storable. A Zusammenpreßen the bobbin during storage, in particular a shrinkage of the bobbin on the Aufspuldom and the formation of a saddle with hard edges and run in middle part should be prevented if possible, so that There are no problems when processing the winding.

According to the invention, the pre-oriented polyester filaments should be simple and manner in a stretch texturing process, especially at high Texturing speeds, preferably greater than 450 m / min, further processed can be. The filaments obtainable by stretch texturing should have excellent material properties, for. B. a high tensile strength of more than 26 cN / tex and a high elongation at break of more than 30% for HE filaments or more than 36% for SET filaments.

These are solved as well as other not explicitly mentioned tasks, however from the contexts discussed hereinbefore readily derivable or be developed by a method for spinning and winding with all Features of claim 1. Advantageous modifications of The method according to the invention are referred to in claim 1 Subclaims under protection. The one obtainable by the spinning process Pre-oriented polyester filament is the independent product claim described. The draw texturing of the preoriented polyester filament becomes claimed in the method claim 6, while the product claims 7 and 8 refer to the bulky filaments obtainable by stretch texturing.

a) der Spinnverzug im Bereich 70 bis 500 eingestellt wird,

b) die Filamente direkt nach Austritt aus der Spinndüse eine Abkühlungsverzögerungszone von 30 mm bis 200 mm Länge durchlaufen,

c) die Filamente unter die Erstarrungstemperatur abgekühlt werden,

d) die Filamente in einem Abstand zwischen 500 mm und 2500 mm von der Düsenunterseite gebündelt werden,

e) die Fadenspannung vor und zwischen den Abzugsgaletten zwischen 0,05 cN/dtex bis 0,20 cN/dtex eingestellt wird, vorzugsweise bis 0,15 cN/dtex,

f) der Faden mit einer Fadenspannung zwischen 0,025 cN/dtex bis 0,15 cN/dtex aufgespult wird,

g) und die Aufspulgeschwindigkeit zwischen 2200 m/min und 3500 m/min eingestellt wird,

gelingt es auf nicht ohne weiteres vorhersehbare Weise vororientierte Polyester-Filamente zur Verfügung zu stellen, die auch nach einer Lagerung bei Normalbedingungen für 4 Wochen ihre hervorragenden Materialeigenschaften bewahren. Eine signifikante Verschlechterung der Gleichmäßigkeitswerte des Fadens infolge einer Alterung bzw. ein Wickelschrumpf der gesponnenen Faser auf der Spule ist nicht zu beobachten.By having at least 90% by weight, based on the total weight of the polyester filament, of polybutylene terephthalate (PBT) and / or polytrimethylene terephthalate (PTMT), preferably of PTMT, of a process for making and winding up preoriented polyester filaments .

a) the spinning delay is set in the range 70 to 500,

b) the filaments go through a cooling delay zone of 30 mm to 200 mm length directly after leaving the spinneret,

c) the filaments are cooled below the solidification temperature,

d) the filaments are bundled at a distance of between 500 mm and 2500 mm from the nozzle base,

e) the yarn tension is adjusted between 0.05 cN / dtex and 0.20 cN / dtex before and between the withdrawal godets, preferably up to 0.15 cN / dtex,

f) the thread is wound with a thread tension between 0.025 cN / dtex to 0.15 cN / dtex,

g) and the winding speed is set between 2200 m / min and 3500 m / min,

It is possible to provide pre-oriented polyester filaments in a manner which can not be foreseen without further ado, which retain their excellent material properties even after storage under normal conditions for 4 weeks. A significant deterioration of the uniformity values of the thread due to aging or winding shrinkage of the spun fiber on the bobbin is not observed.

⇒ Das erfindungsgemäße Verfahren ist auf einfache Art und Weise, großtechnisch und kostengünstig durchführbar. Insbesondere erlaubt das Verfahren das Spinnen und Aufspulen bei hohen Abzugsgeschwindigkeiten von mindestens 2200 m/min und die Herstellung hoher Fadengewichte auf dem Spulkörper von mehr als 4 kg.

⇒ Durch das Verfahren der vorliegenden Erfindung kann auf den Einsatz von Spinnadditiven verzichtet werden. Hierdurch können Polyester-Filamente besonders kostengünstig erhalten werden.

⇒ Die durch das Verfahren erhältlichen vororientierten Polyester-Filamente können somit auf einfache Art und Weise, großtechnisch und kostengünstig in einem Streck- bzw. einem Strecktexturierprozeß weiterverarbeitet werden. Dabei kann die Texturierung bei Geschwindigkeiten größer 450 m/min erfolgen.

⇒ Aufgrund der hohen Gleichmäßigkeit der durch das Verfahren erhältlichen vororientierten Polyester-Filamente ist es auf einfache Art und Weise möglich, einen guten Spulenaufbau einzustellen, der eine gleichmäßige und nahezu fehlerfreie Anfärbung und Weiterverarbeitung des vororientierten Polyester-Filaments erlaubt.

⇒ Die durch die Strecktexturierung erhältlichen Filamente weisen eine hohe Reißfestigkeit von mehr als 26 cN/tex und eine hohe Reißdehnung von mehr als 30 % für HE-Filamente bzw. mehr als 36 % für SET-Filamente auf.

At the same time, the inventive method has a number of other advantages. These include:

⇒ The method according to the invention can be carried out in a simple manner, on an industrial scale and at low cost. In particular, the method allows spinning and winding at high take-off speeds of at least 2200 m / min and the production of high thread weights on the bobbin of more than 4 kg.

⇒ By the method of the present invention can be dispensed with the use of spin additives. As a result, polyester filaments can be obtained particularly inexpensively.

⇒ The preoriented polyester filaments obtainable by the process can thus be further processed in a simple manner, industrially and inexpensively in a stretch or a draw texturing process. The texturing can take place at speeds greater than 450 m / min.

⇒ Due to the high uniformity of the pre-oriented polyester filaments obtainable by the process, it is possible in a simple manner to set a good package structure which permits a uniform and virtually error-free dyeing and further processing of the preoriented polyester filament.

⇒ The filaments obtainable by stretch texturing have a high tensile strength of more than 26 cN / tex and a high elongation at break of more than 30% for HE filaments or more than 36% for SET filaments.

The present invention relates to a process for the production and for winding preoriented polyester filaments which are at least 90 Wt .-% based on the total weight of the filament Polybutylene terephthalate (PBT) and / or polytrimethylene terephthalate (PTMT) consist. Polybutylene terephthalate (PBT) and / or polytrimethylene terephthalate (PTMT) are known in the art. Polybutylene terephthalate (PBT) can by Polycondensation of terephthalic acid with equimolar amounts of 1,4-butanediol, Polytrimethylene terephthalate by polycondensation of Terephthalic acid with equimolar amounts of 1,3-propanediol can be obtained. Also mixtures of the two polyesters are conceivable. According to the invention preferred becomes PTMT.

The polyesters can be both homopolymers and copolymers. As copolymers In particular, those in question, in addition to recurrent PTMT and / or PBT units still up to 15 mol% based on all Repeating units of polyester repeating units more usual Comonomers, such as. Example, ethylene glycol, diethylene glycol, triethylene glycol, 1,4-cyclohexanedimethanol, Polyethylene glycol, isophthalic acid and / or adipic acid, contain. In the context of the present invention, however, polyester homopolymers prefers.

The polyesters according to the invention can be customary amounts other additives than admixtures, such as catalysts, stabilizers, Antistatic agents, antioxidants, flame retardants, dyes, dye-uptake modifiers, Light stabilizers, organic phosphites, optical brighteners and Matting agents included. Preferably, the polyesters contain 0 to 5 wt .-% based on the total weight of the filament of additives.

Furthermore, the polyesters can also a small proportion, preferably up to 0.5 wt .-% based on the total weight of the filament, on Branching components, included. To the inventively preferred Branching components include polyfunctional acids, such as Trimellitic acid, pyromellitic acid, or tri- to hexavalent alcohols, such as Trimethylolpropane, pentaerythritol, dipentaerythritol, glycerol, or the like Hydroxy acids.

The usable according to the invention polyesters are preferably thermoformable and can be spun into filaments and spooled become. In this case, such polyesters are particularly advantageous, the one Intrinsic viscosity in the range of 0.70 dl / g to 0.95 dl / g.

In the method according to the invention is a melt or melt mixture the polyester by means of spinning pumps at a constant speed, the speed is set according to known formula, that the desired yarn titer is obtained, pressed into nozzle packages and through the nozzle holes of the nozzle plate of the package is extruded into molten filaments.

The melt can be made for example in an extruder of polymer chips are, where it is particularly favorable, the chips previously on a water content ≤ 30 ppm, in particular to a water content of ≤ 15 ppm.

T_m:

Schmelzpunkt des Polyesters [°C]

T_Sp:

Spinntemperatur [°C].

The temperature of the melt, which is commonly referred to as the spinning temperature and measured in front of the spinning pump, depends on the melting point of the polymer used or the polymer mixture used. It is preferably in the range given by formula 1: Formula 1: T m + 15 ° C ≤ T sp ≤ T m + 45 ° C With

T _m:

Melting point of the polyester [° C]

T _Sp :

Spinning temperature [° C].

The specified parameters serve to limit the hydrolytic and / or thermal viscosity degradation, the expediently as possible should be low. In the context of the present invention is a viscosity reduction less than 0.12 dl / g, in particular less than 0.08 dl / g, desirable.

The homogeneity of the melt has a direct influence on the Material properties of the spun filaments. Preferably used therefore a static mixer with at least one element, which after the Spinning pump is installed, for homogenization of the melt.

The temperature dependent on the spinning temperature of the nozzle plate is through regulated their so-called heat tracing. Come as a heat For example, a "Diphyl" heated spinning beam or additional Convection or radiant heater in question. Usually the temperature is the nozzle plates at the level of spinning temperature.

An increase in temperature at the nozzle plate can be due to the pressure gradient in the Nozzle package can be achieved. Known derivations, such as K. Riggert "Advances in the Production of Polyester Tire Cord Yarn" Chemical Fibers 21, Page 379 (1971) describe a temperature increase of about 4 ° C per 100 bar pressure drop.

Furthermore, it is possible to increase the nozzle pressure by using loose filter media, in particular of steel sand with a mean grain size between 0.10 mm and 1.2 mm, preferably between 0.12 mm and 0.75 mm and / or filter blanks, the made of metal fabrics or non-wovens with a fineness ≤ 40 μ can control.

In addition, the pressure drop in the nozzle hole contributes to the total pressure. Of the Nozzle pressure is preferably between 80 bar and 450 bar, in particular set between 100 bar and 250 bar.

δ:

Dichte der Schmelze [g/cm³]; für PTMT = 1,12 g/cm³

D:

Düsenlochdurchmesser [cm]

dpf:

Titer des Einzelfilamentes [den]

The spinning distortion i _Sp , ie the quotient of take-off speed and injection speed, is calculated according to US Pat. No. 5,250,245 via formula 2 with the density of the polymer or polymer mixture, the nozzle hole diameter and the titer of the single filament: Formula 2: i sp = 2.25 • 10 5 • (δ • π) • D 2 (Cm) / dpf (denier) With

δ:

Density of the melt [g / cm ³ ]; for PTMT = 1.12 g / cm ³

D:

Nozzle hole diameter [cm]

dpf:

Titre of the individual filament

In the context of the present invention, the spinning delay is between 70 and 500, preferably between 100 and 250.

The length / diameter ratio of the nozzle hole is preferably between 1.5 and 6 selected, in particular between 1.5 and 4.

The extruded filaments pass through a cooling delay zone. Directly below the nozzle package this is formed as a return zone, in the emerging from the nozzle holes filaments before the direct action the cooling gas to be stored and delayed in delay or cooling. An active part of the return is as an offset of the nozzle package in the Spinning beam carried out so that the filaments of heated walls are surrounded. A passive part is through insulation layers and unheated Frame formed. The lengths of the active return are between 0 and 100 mm, that of the passive part between 20 to 120 mm, with a total length of 30 - 200 mm, preferably 30 - 120 mm is maintained.

As an alternative to the active recess may be below the spinner Be installed reheater. In contrast to the active return points then this zone of cylindrical or rectangular cross section at least a heating independent of the spinning beam

For radial, the thread concentrically surrounding porous cooling systems can the cooling delay achieved by means of cylindrical covers become.

Subsequently, the filaments are at temperatures below their Solidification temperature cooled. According to the invention denotes the Solidification temperature is the temperature at which the melt in the solid State of aggregation passes.

In the context of the present invention, it has proven to be particularly useful proved to cool the filaments to a temperature at which they in essential are no longer sticky. Particularly advantageous is a cooling the filaments to temperatures below their crystallization temperature, in particular to temperatures which are below their glass transition temperature.

Means for cooling the filaments are those skilled in the art from the Technique known. The use has proven particularly useful according to the invention of cooling gases, in particular cooled air. The cooling air points preferably a temperature of 12 ° C to 35 ° C, especially 16 ° C to 26 ° C. on. The speed of the cooling air is advantageously in the range of 0.20 m / sec to 0.55 m / sec.

For example, monofilament systems can be used to cool the filaments used, consisting of individual cooling tubes with perforated wall consist. Through active cooling air supply or by using the Self-priming effect of the filaments becomes a cooling each achieved single filament. Alternative to the single tubes are also the known Querstromanblasungssysteme used.

A special embodiment of the cooling and drafting area exists therein, the filaments emerging from the retarding zone in a zone of the Length in the range of 10 to 175 cm, preferably in a zone of length in Range of 10 - 80 cm to supply cooling air. It is for filaments with a Titer when winding ≤ 1.5 dtex per filament a zone length in the range of 10 - 40 cm and for filaments with a titer between 1.5 and 9.0 dtex per Filament a zone length in the range of 20 - 80 cm particularly suitable. it then the filaments and their accompanying air through a cross-section reduced channel passed together, being controlled by the Cross-sectional tapering and dimensioning in the thread running direction Ratio of air to yarn speed when peeling from 0.2 to 20: 1, preferably 0.4 to 5: 1, is set.

After cooling the filaments to temperatures below the Solidification temperature, they are bundled into a thread. Of the According to the invention suitable distance of the bundling of the nozzle bottom can by methods known to those skilled in the art for online measurement of Thread speed and / or thread temperature, for example with a Laser Doppler anemometer from TSI / D or an infrared camera of the company Manufacturer Goratec / D type IRRIS 160, to be determined. He is 500 to 2500 mm, preferably 500 to 1800 mm. This filaments are with a Titer ≤ 3.5 dtex, preferably at a smaller distance ≤ 1500 mm, thicker Filaments are preferably bundled at a greater distance.

In the context of the present invention, it is expedient that preferably all Surfaces that come into contact with the spun filament from particularly low-friction materials are made. In this way linting can be largely avoided, it will be higher quality Obtained filaments. As especially suitable for this purpose low-friction surfaces of the specification "TriboFil" from the company Ceramtec / D proven.

The bundling of the filaments takes place in an oiler stone, the thread the the desired amount of spin finish uniformly. A special suitable Ölerstein is characterized by an inlet part, the thread channel with oil inlet opening and the outlet part. The inlet part is funnel-shaped extended so that contact with the still-dry filaments avoided becomes. The impact point of the filaments takes place within the thread channel the inflow of the preparation. Thread channel and oil inlet opening are in the Width adapted to the thread titer and the number of filaments. Particularly well proven have openings and widths in the range of 1.0 mm to 4.0 mm. Of the Outlet part of the oiler is designed as a homogenization distance, the preferably has oil reservoirs. Such oilers can, for example, from the Company Cermatec / D or Goulston / USA.

The uniformity of the oil application can according to the invention of great importance be. It can, for example, with a Rossa meter according to the in Chemical fibers / textile industry, 42./94, Nov. 1992 on page 896 described Method to be determined. Preferably, in such Procedure Values for the standard deviation of the oil application of less obtained as 90 digits, in particular less than 60 digits. According to the invention Particular preference is given to values for the standard deviation of the oil application less than 45 digits, in particular less than 30 digits. there corresponds to a value for the standard deviation of 90 digits or 45 digits about 6.2% and 3.1% of the coefficient of variation, respectively.

In the context of the present invention, it has proven to be particularly advantageous proved self-degassing lines and pumps to avoid gas bubbles interpreted, as these can lead to a significant oil application fluctuation.

According to the invention, an entangling is particularly preferred before being wound up Thread. Here are nozzles with closed yarn channels as special proved suitable, since in such systems entanglements of the thread in the Insertion slot avoided even with low thread tension and high air pressure become. The Entanglingdüsen are preferably between godets arranged, wherein the exit thread tension by means of different Speed of the inlet and outlet galette is regulated. It should be .20 cN / dtex and primarily values between 0.05 cN / dtex and 0.15 cN / dtex. The air pressure of Entanglingluft is between 0.5 and 5.5 bar, at winding speeds up to 3500 m / min at a maximum of 3.0 bar.

Preferably, node numbers of at least 10 n / m are set. there are maximum opening lengths less than 100 cm and values for the Coefficients of variation of the number of nodes below 100% of particular Interest. Advantageously, when using air pressures above 1.0 bar nodal numbers ≥ 15 n / m achieved by a high uniformity characterized in that the coefficient of variation is less than or equal to 70% and the maximum opening length is 50 cm. In practice, systems have become of the type LD of the company Temco / D, the double system of the company Slack & Parr / USA, or nozzles of the type Polyjet of Heberlein as proved particularly suitable.

The peripheral speed of the first godet unit is called Discharge speed called. Other godet systems can be used be before the thread in the winding unit to winding bodies (coils) on Sleeves is wound up.

Stable, error-free filament wound bodies are a prerequisite for error-free removal of the thread and for as error-free as possible Further processing. Therefore, in the context of the present process, a Winding tension in the range of 0.025 cN / dtex - 0.15 cN / dtex, preferably in Range of 0.03 cN / dtex - 0.08 cN / dtex.

An important parameter of the inventive method is the setting of Thread tension before and between the withdrawal godets. As is known, it is this voltage essentially from the actual orientation voltage Hamana, the friction tension on the yarn guides and the oiler and the Thread-air friction tension together. In the context of the present Invention is the thread tension before and between the withdrawal godets in Range from 0.05 cN / dtex to 0.20 cN / dtex, preferably between 0.08 cN / dtex and 0.15 cN / dtex.

Too low a tension below 0.05 cN / dtex will no longer give the desired level of preorientation. If the stress exceeds 0.20 cN / dtex, then This voltage releases a memory effect when winding and storing the coils out, which leads to the deterioration of the thread characteristics.

According to the invention, the tension is determined by the oiler distance from the nozzle, the Friction surfaces and the length of the distance between oiler and withdrawal godet regulated. This route length is advantageously not more than 6.0 m, preferably less than 2.0 m, with the spinning and drawing machine are arranged by parallel construction such that a straight yarn path is guaranteed.

The geometric parameters also change the conditioning time of the thread between bundling point and Aufspulung described. The fast-running Relaxation during this time affects the quality of the coil construction. Preferably, the conditioning time defined in this way is between 50 and 200 ms selected.

The winding speed of the POYs is between 2200 according to the invention m / min and 3500 m / min.

Advantageously, during the implementation of the inventive Method in the vicinity of the thread winding a temperature ≤ 45 ° C, especially between 12 and 35 ° C, and a relative humidity of 40 - 85% set. The storage of the POY until further processing is preferred at a temperature ≤ 45 ° C. Furthermore, it is expedient the POY coils at least 4 hours at 12 to 35 ° C and a relative humidity of 40-85% store before further processing.

a) eine Reißdehnung zwischen 90 und 165 %, vorzugsweise zwischen 90 und 135 %

b) einen Kochschrumpf von mindestens 30 %, vorzugsweise ≥ 40%,

c) einen Normal-Uster unterhalb von 1,1 %, vorzugsweise kleiner 0,9 %,

d) eine Doppelbrechung zwischen 0,030 und 0,058,

e) eine Dichte kleiner 1,35 g/cm³, vorzugsweise kleiner 1,33 g/cm³,

f) einen Variationskoeffizienten der Reißlast ≤ 4,5 %, vorzugsweise ≤ 2,5 % und

g) einen Variationskoeffizienten der Reißdehnung ≤ 4,5 %, vorzugsweise ≤ 2,5 % auf.

The filament of the invention has after 4 weeks storage under normal conditions

a) an elongation at break between 90 and 165%, preferably between 90 and 135%

b) a boiling shrinkage of at least 30%, preferably ≥ 40%,

c) a normal Uster below 1.1%, preferably below 0.9%,

d) a birefringence between 0.030 and 0.058,

e) a density of less than 1.35 g / cm ³ , preferably less than 1.33 g / cm ³ ,

f) a coefficient of variation of the breaking load ≤ 4.5%, preferably ≤ 2.5% and

g) a coefficient of variation of the elongation at break ≤ 4.5%, preferably ≤ 2.5%.

The term "normal conditions" is known to those skilled in and over the Standard DIN 53802 defined. Under "normal conditions" according to DIN 53802 the temperature is 20 ± 2 ° C and the relative humidity 65 ± 2%.

In addition, it is particular in the context of the present invention advantageous in that the boiling shrinkage measured directly after being wound up between 50 and 65% and after 4 weeks storage under normal conditions at least 30%, preferably ≥ 40%. Surprisingly, it has become have shown that POY coils produced in this way are excellent for further processing to let.

It should be noted that in practice climate conditions at the production, storage or transport of the POY is not always can be complied with. With low crystalline thread, however, occurs frequently the problem is that the POY coils change in shape, the Draw ratio and / or the texturing speed must be reduced and in subsequent processing more fractures occur. Yarns that comply with the above-mentioned specifications of the cooking shrink, have such Problems compared to conventional yarns on a reduced scale.

In addition, it can be seen that preferred yarns of the present invention also for a storage period of 2 months, no changed staining depth of the DTY exhibit. After a storage period of 20 months, the color change is within 95 ± 3% as long as the ambient temperature is not higher than 45 ° C.

Furthermore, preferred filaments have a natural one Draw ratio greater than or equal to 15%. Particularly preferred is this size ranges from 18 to 65%. The higher the natural Draw ratio is, the better the stretchability. At the same Elongation becomes higher at a high natural draw ratio Draw ratio achieved.

The natural draw ratio is defined as the plateau section in FIG Percent of the force-strain diagram. This size is known and will be published on Tear unit in one operation to determine strength and elongation determined.

FIGS. 2 a) and 2 b) show schematically the indicated parameter of FIG natural draw ratio (NVV), being the natural Draw ratio in Figure 2 b) is zero. It is stated in the diagrams each force versus elongation, with schematic diagrams shown are to explain the parameter in more detail.

It is believed that the natural draw ratio is a measure of the Thread orientation is and a value of NVV <15% is incipient crystallization of the polyester. Low NVV values are e.g. by thermal Treatment of the thread until winding with temperatures of at least 8 ° C above the glass transition temperature of the PES.

Method for determining the specified material parameters are the Professional well known. They can be taken from the specialist literature. Although most parameters are determined in different ways In the context of the present invention, the following methods for determining the filament characteristics as particularly useful:

The intrinsic viscosity is in the capillary viscometer from Ubbelohde at 25 ° C and calculated according to known formula. As a solvent is a Mixture of phenol / 1,2-dichlorobenzene in the weight ratio 3: 2 used. The Concentration of the solution is 0.5 g of polyester per 100 ml of solution.

To determine the melting point, the crystallization and the glass transition temperature a calorimeter DSC device from Mettler is used. Here is the Sample first heated to 280 ° C and melted and then quenched. The DSC measurement is carried out in the range of 20 ° C to 280 ° C with a heating rate of 10 K / min. The temperature variables are determined by the processor.

The determination of the density of filaments is carried out in a density-gradient column at a temperature of 23 ± 0.1 ° C. The reagent used is n-heptane (C ₇ H ₁₆ ) and tetrachloromethane (CCl ₄ ). The result of the density measurement can be used to calculate the degree of crystallinity, based on the density of the amorphous polyester D _a and the density of the crystalline polyester D _k . The corresponding calculation is known from the literature, for example for PTMT D _a = 1.295 g / cm ³ and D _k = 1.429 g / cm ³ .

The titer is known with a precision grape and a weighing device in Determined way. The bias is suitably for Preoriented filaments (POYs) 0.05 cN / dtex and for textured yarn (DTY) 0.2 cN / dtex.

Tear strength and elongation at break are included in a Statimat meter the following conditions are determined; the clamping length is 200 mm for POY or 500 mm for DTY, the measuring speed is 2000 mm / min for POY or 1500 mm / min for DTY, the preload is 0.05 cN / dtex for POY or 0.2 cN / dtex for DTY. By dividing the values for the maximum breaking load the titer determines the tear strength and the elongation at break is added evaluated maximum load.

Strands of filaments are used to determine the boiling shrinkage de-energized in water at 95 ± 1 ° C for 10 ± 1 min. The strands are tempered with a bias of 0.05 cN / dtex for POY or 0.2 cN / dtex for DTY produced; the length measurement of the strands before and after the temperature treatment takes place at 0.2 cN / dtex. From the Length difference is calculated in a known manner of boiling shrinkage.

The determination of the birefringence is carried out according to the in DE 19,519,898 described procedure. Therefore, explicit in this context the disclosure of DE 19,519,898 reference.

The crimp characteristics of the textured filaments are in accordance with DIN 53840, Part 1 with the texturates of the company Stein / D at 120 ° C development temperature measured.

The normal Uster values are determined with the Uster tester 4-CX and as Uster% values indicated. It is at a test speed of 100 m / min the test time 2.5 min.

The POY according to the invention can be further processed in a simple manner, in particular stretch texturized. In the context of the present invention the stretch texturing preferably takes place at a texturing speed of at least 500 m / min, more preferably in one Texturing speed of at least 700 m / min. The draw ratio is preferably at least 1: 1.35, in particular at least 1: 1.40. It has become Stretch texturing on a high temperature heater type machine, such as For example, the AFK the company Barmag, proved to be particularly useful.

The bulky filaments thus produced have a low number Lint and after staining under cooking conditions at 95 ° C with a Dispersion dye (Terasil Navy Blue) without carrier an excellent color depth and color uniformity.

Bulky SET filaments produced according to the invention preferably have a tensile strength of more than 26 cN / tex and an elongation at break of more than 36%. For bulky HE filaments, the without temperature application in one second heaters are available, the tear strength is preferably more than 26 cN / tex and the elongation at break more than 30%.

The bulking and elasticity behavior of the filaments according to the invention is outstanding.

The invention will be explained in more detail by examples, without the invention should be limited to these examples.

Examples 1 and 2 Spinning and winding

PTMT chips with an intrinsic viscosity of 0.93 dl / g, a melt viscosity of 325 Pa s (measured at 2.4 Hz and 255 ° C), a melting point of 227 ° C, a crystallization temperature of 72 ° C and a glass transition temperature from 45 ° C were dried at a temperature of 130 ° C in a tumble dryer to a water content of 11 ppm.
The chips were melted in a Barmag 3E4 extruder so that the temperature of the melt was 255 ° C. It was then fed to the spin pump through a product line containing a Sulzer SMX 15-element static mixer with an inner diameter of 15 mm. The transported amount of melt was 63 g / min with a residence time of 6 min, the amount added by the spin pump to the nozzle pack was 30.7 g / min. After the spinning pump before entering the nozzle package, an element static mixer, type HD-CSE with 10 mm inner diameter of Fluitec was installed. The product line and spinner block heaters containing the pump and nozzle pack were set at 255 ° C. The nozzle package contained steel sand with a grain size of 350-500 μm with a height of 30 mm and a 20 μm nonwoven and a 40 μm fabric filter as filter media. The melt was extruded through a die plate of 80 mm diameter and 34 holes of 0.25 mm diameter and 1.0 mm length. The nozzle pressure was 120 bar.

The cooling delay zone had a length of 100 mm, with 30 mm heated wall and 70 mm insulation and unheated frame were. The Melt filaments were then subsequently in a blow shaft with Querstromanblasung a blow length of 1500 mm cooled. The cooling air had a speed of 0.35 m / sec, a temperature of 18 ° C and a relative Humidity of 80%. The solidification point of the filaments was at a distance of 800 mm below the spinneret.

With the help of a thread oiler at a distance of 1050 mm from the nozzle were provided the threads with spin finish and bundled. The oiler was with one TriboFil surface and had an inlet opening of 1 mm Diameter. The applied preparation amount was 0.40% based on the Thread weight.

The bundled thread was then fed to the winding machine. The distance between oiler and first withdrawal godet was 3.2 m. The conditioning time was depending on the speed 144 or 168 ms. A pair of godets became S-shaped from the thread entwined. Between the godets was a Temco Entangling nozzle installed, which was operated with an air pressure of 1.5 bar. According to the Speed setting was the winding speed of the winder of the type SW6 of the company Barmag adjusted so that the Aufspilladenspannung 5 cN. The indoor climate was at 24 ° C at 60% Relative humidity adjusted so that in the environment of the Filament winding set a temperature of about 34 ° C.

In the context of the present experiments, the take-off speed was either 2940 m / min (Example 1) or 2506 m / min (Example 2). Table 1 shows the other experimental parameters, Table 2, the material properties of the resulting pre-oriented filaments (POYs) again. With both settings, coil weights of 10 kg could be produced and removed without problems from the winding spool of the winder. experimental parameters experimental parameters example 1 Example 2 off speed [M / min] 2940 2506 winding speed [M / min] 2926 2500 spinning draft 178 152 thread tensions in front of godets [CN] 14 10 between godets Max [CN] 11 7.5 in front of godets [CN / dtex] 0.13 0.08 between godets Max [CN / dtex] 0.10 0.06 Aufspulfadenspannung [CN] 5.0 5.0 Aufspulfadenspannung [CN / dtex] 0.048 0,041 Material properties of the preoriented PTMT filaments material properties example 1 Example 2 titres [Dtex] 105 123 tear strength [CN / tex] 23.4 20.7 elongation at break [%] 98 127 Normal Uster [%] 0.9 0.76 boiling shrinkage [%] 46 33 Birefringence • 10 ³ .DELTA.n 52 43 density [g / cm ³ ] 1,320 1,318 CV-breaking load [%] 2.2 1.9 CV elongation at break [%] 2.2 1.9

drawtexturizing

The PTMT filament coils were exposed to normal climate for four weeks according to DIN 53802 and then a draw texturing machine from Barmag, type FK6-S-900, submitted. The experimental parameters of stretch texturing for Production of so-called SET filaments are shown in Table 3, which Material properties of the resulting bulky SET filaments are in Table 4 summarized.

The texturing errors were detected by UNITENS of the Fima Barmag at the following limit settings: UP / LP = 3.0 cN, UM / LM = 6.0 cN. Experimental parameters of stretch texturing experimental parameters example 1 Example 2 speed [M / min] 700 700 draw ratio 1: 1.48 1: 1.65 D / Y-ratio 2.1 2.1 Temp. Heater 1 [° C] 155 155 Temp. Heater 2 [° C] 160 160 Texturierfehler [n / 10 km] 0 0 thread tension F ¹ before aggregate [CN] 20 20 F , after aggregate [CN] 19 18 F -CV [%] 1.2 1.3 Material properties of the stretch-textured filaments material properties example 1 Example 2 titres [Dtex] 78 82 tear strength [CN / tex] 27.7 29.0 elongation at break [%] 39.4 39.9 visual staining assessment evenly evenly curling [%] 85 87 crimp [%] 24.5 25

By a cold mode of the 2nd heater, d. H. by the production of so-called HE filaments, the bulk behavior can be varied. The crimping then increases to about 47%. The elongation at break then drops to 33%.

Claims (8)

1. A process for producing and winding POY polyester filaments not less than 90% by weight, based on the total weight of the polyester filament, polybutylene terephthalate (PBT) and/or polytrimethylene terephthalate (PTMT), preferably PTMT, characterized in that it comprises

   a) setting the spinline extension ratio in the range from 70 to 500,

   b) passing the filaments directly upon exit from the spinneret through a quench delay zone 30 mm to 200 mm in length,

   c) quenching the filaments to below the solidification temperature,

   d) converging the filaments at a distance between 500 mm and 2 500 mm from the underface of the spinneret,

   e) setting the yarn tension above and between the takeoff godets between 0.05 cN/dtex to 0.20 cN/dtex,

   f) taking the yarn up at a yarn tension between 0.025 cN/dtex to 0.15 cN/dtex,

   g) setting the takeup speed between 2 200 m/min and 3 500 m/min.
2. A process as claimed in claim 1, characterized in that PBT and/or PTMT having a limiting viscosity number in the range from 0.7 dl/g to 0.95 dl/g are used.
3. A process as claimed in claim 1 and/or 2,
   characterized in that the taking up is effected by setting a temperature ≤ 45°C in the ambience of the yarn package.
4. A process as claimed in at least one of the preceding claims, characterized in that the POY bobbins are stored at 12-35°C and 40-85% relative humidity for at least 4 hours prior to further processing.
5. POY polyester filaments obtainable by a process as claimed in at least one of the preceding claims, characterized in that it has

   a) a breaking extension between 90% and 165%,

   b) a boiloff shrinkage of at least 30%,

   c) a normal Uster below 1.1%,

   d) a birefringence between 0.030 and 0.058,

   e) a density of less than 1.35 g/cm³, preferably less than 1.33 g/cm³,

   f) a breaking load coefficient of variation ≤4.5% and

   g) a breaking extension coefficient of variation ≤4.5%

   after 4 weeks of storage under standard conditions as defined in DIN 53802.
6. A process for producing bulky polyester filaments, characterized in that filaments as claimed in claim 5 are processed in a draw-texturing machine at a speed of at least 500 m/min and a draw ratio of at least 1.35:1 into a bulky yarn.
7. Bulky polyester SET filaments obtainable by a process as claimed in claim 6, characterized in that their breaking strength is more than 26 cN/tex and the breaking extension more than 36%.
8. Bulky polyester HE filaments obtainable by a process as claimed in claim 6, characterized in that their breaking strength is more than 26 cN/dtex and the breaking extension more than 30%.

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