CN1306083C - Method for spinning and reeling polyester multifilament yarns by using spinning additives, and polyester multifilament yarns obtained by said spinning method - Google Patents

Abstract

The invention relates to a method for producing and reeling pre-oriented polyester multifilament yarns comprising polybutylene terephthalate (PBT) and/or polytrimethylene terephthalate (PTMT) at a proportion of at least 85 percent by weight relative to the total weight of the multifilament yarn and at least one additive polymer at a proportion ranging between 0.05 percent by weight and 2.5 percent by weight relative to the total weight of the multifilament yarn as a stretch-increasing means. The inventive method is characterized by the fact that a wound thread package is supplied which displays long-term stability during storage and is insensitive to elevated temperatures during storage and transport by heat-treating the wound thread package of the polyester multifilament yarn at a temperature ranging from > 45 DEG C to 65 DEG C. The invention also relates to polyester multifilament yarns obtained by the inventive method and the use thereof.

Description

Spinning and winding of polyester multifilament yarn using spinning additives and use of polyester multifilament yarn obtainable by the method

The present invention relates to a method for spinning and winding polyester monofilaments and also to polyester multifilaments obtainable by this method, based on the total weight of polyester monofilaments not less than 85% by weight is polybutylene terephthalate (PBT) and/or polytrimethylene terephthalate (PTMT), preferably PTMT. The invention also relates to the use of polyester multifilaments for drawtexturing.

The two-stage production of continuous polyester multifilaments, in particular polyethylene terephthalate (PET) multifilaments, is known. In this method, the first step involves spinning and winding the multifilaments that are fully drawn and heat-set or stretch-textured into a bulky multifilament yarn in the second step. The coils of wound multifilament yarn can be stored for long periods of time and transported at relatively high temperatures between the two steps, which would otherwise have an impact on the processing conditions of the second step or the quality of the obtainable product .

A review of this field is Synthetische Fasern (1995) by F. Fourné, Hanser, Munich. The basic principles of spinning and winding are described in this book.

However, unlike PET multifilament yarns, polytrimethylene terephthalate (PTMT) or polybutylene terephthalate (PBT) multifilament yarns are not only After winding, but also within hours and days after winding, during storage and transportation, especially at relatively high ambient temperatures, it shows a fairly significant tendency to shrink, which leads to yarn shorten. As a result, the roll is compressed and in extreme cases the roll will shrink firmly onto the winding mandrel and can no longer be removed. During prolonged storage or during transport, especially at elevated temperatures, wound yarn reels lose their desired "cheese-like" structure and develop so-called hard edges and waists. A saddle at the center of the shape. As a result, the spinning data of the multifilament deteriorates and problems arise when unwinding the coil. The problems that do not arise with the handling of these PET fibers can generally only be avoided by limiting the weight of the yarn reels to less than 2 kg.

It was also observed that, unlike PET multifilaments, PBT or PTMT multifilaments age rapidly during storage. It is more observable at ambient temperatures equal to and above the glass transition temperature range of the polymer. Structural hardening occurs and causes the properties of the multifilament to change over time, such as reduced desizing shrinkage. However, industrial practice requires storage-stable multifilaments with constant yarn properties, which are independent of specific storage conditions and allow continuous further processing to obtain multifilaments with uniform properties.

Differences between PET and PBT and PTMT are often attributed to differences in structure and properties, as reported in Chemical Fibers Int. Vol. 50, p. 53 (2000) and held in Dornbirn, 13-15 September 2000 Discussed at the 39th International Manmade Fibers Congress. From this it is believed that the different chain formation and higher glass transition temperature of PET and PTMT/PBT are responsible for the difference in properties.

The first attempts to solve these problems are described in patent applications WO 99/27168, WO01/04393 and European patent EP 0731196 B1. WO 99/27168 discloses the production of polyester multifilaments by spinning and drawing not less than 90% by weight of PTMT. The reported maximum spinning takeoff speed (takeoff speed) is 2100m/min, but from an economic point of view, this speed is too low. The polyester multifilaments obtained by this method have a desizing shrinkage between 5% and 16% and an elongation at break between 20% and 60%, so their use for further processing is limited because of the low Elongation at break represents a large number of processing defects during further processing. Additionally, the resulting yarn will have a reduced breaking tenacity.

WO 01/04393 relates to a method for producing PTMT multifilaments in which the multifilaments are heat treated with a heated godet. The article is silent on storage or transport stability, especially at relatively high temperatures. A disadvantage of this method is that it requires a low spinning take-off speed. Economically desirable speeds increase the necessity for shorter contact times of the multifilaments with the heated godets, which leads to long-term storage stability of the resulting yarn reels and changes in POY desizing shrinkage at relatively high temperatures. bad.

European patent EP 0731196 B1 claims a method of spinning, drawing and winding for synthetic yarns by heat treating the yarn after drawing and before winding to reduce its tendency to shrink. Useful synthetic fibers are polytrimethylene terephthalate fibers. In EP 0731196 B1 heat treatment is achieved by introducing synthetic yarns along an elongated heating surface in close but substantially no contact. The handling of yarn reels is not described in the reference. There are also no references showing any information concerning storage stability and transport stability of wound yarn reels.

Another frequently observed problem during the spinning and winding of multifilament yarns, especially at high speeds, is annoying noise, especially near the winder. For this reason, it has already been proposed to incorporate the winder device into a soundproof housing. However, the thermal treatment of wound yarn reels within an acoustic enclosure has not hitherto been described in the prior art.

It is therefore an object of the present invention to solve the above-mentioned problems. In particular, it is an object of the present invention to provide a method for spinning and winding polyester multifilament yarns based on a total weight of monofilaments, PBT and/or PTMT of not less than 85% by weight, whereby it is possible and simple Production and winding of polyester multifilament yarns. With regard to the parameters of the monofilaments, the polyester multifilament should have an elongation at break of >60%, preferably 75%-145%, a desizing shrinkage of 0-10%, and a high uniformity.

Another object of the present invention is to provide an economical industrial process for spinning and winding polyester multifilament yarns. The method of the invention should allow very high spinning draw-off speeds, preferably higher than 2200 m/min, and yarn weights on the reel greater than 2 kg, especially greater than 4 kg, the wound yarn reels should advantageously be in uniform bobbins Yarn-like, free from raised and flaking strands.

A further object of the invention is to improve the storage stability of the polyester multifilaments obtained by the process of the invention. They should be storable for a long time, eg 4 weeks. Ideally, during storage, the roll should not compress, especially not shrink firmly onto the winding mandrel and form a saddle shape with hard edges and a waist-like middle section, so unwinding from the yarn roll should not occur. will be a problem.

According to the invention, the polyester multifilaments will be easily subjected to further drawing or drawing texturing operations, especially at high texturing speeds, preferably higher than 450 m/min. Multifilament yarns obtained by stretch texturing should possess excellent material properties such as high breaking tenacity and elongation at break, low filament breakage and uniform dyeability.

These and other objects not explicitly mentioned, but which can be easily derived or become apparent from the related matters discussed at the outset, can be achieved by a process of spinning and winding which is characterized by: Process for winding partially oriented polyester multifilament yarns containing not less than 85% by weight of polybutylene terephthalate (PBT) and/or poly 1,3-Trimethylene terephthalate (PTMT), containing 0.05% to 2.5% by weight, based on the total weight of the multifilament yarn, of at least one polymeric extensibility enhancer as an additive, the method Including providing wound yarns which are stable for long term storage and insensitive to elevated temperatures during storage and transport by heat treating wound polyester multifilament yarn rolls at temperatures ranging from greater than 45°C to 65°C roll. Beneficial modifications of the method according to the invention are also protected in the claims of the present application. Also described in the claims of the present application are polyester multifilament yarns obtainable by the spinning process, as well as stretch texturing of partially oriented polyester monofilaments and bulky monofilaments obtainable by stretch texturing. Thus, the present invention provides a method for producing and winding polybutylene terephthalate (PBT) and/or polyterephthalic acid containing not less than 85% by weight (based on the total weight of the multifilament yarn) of polybutylene terephthalate (PBT) and/or polyterephthalic acid. - Process for polyester multifilaments of 1,3-propanediol ester (PTMT) and 0.05% to 2.5% by weight (based on the total weight of the multifilament yarn) of at least one polymeric extensibility enhancer additive by Long-term storage stability and insensitive to elevated temperature during storage and transportation, the winding yarn package is carried out by winding polyester multifilament yarn at > 45 ° C to 65 ° C obtained by heat treatment at a temperature of °C.

This unexpected approach provides polyester multifilaments that retain their excellent material properties even after 4 weeks of storage, especially after storage and transport at relatively high temperatures up to 65°C. No significant deterioration in the consistency rating of the yarn due to aging and no shrinkage of the spun fibers on the spool was observed.

At the same time, the method of the invention has many other advantages. These include:

→The method of the present invention can be used in large-scale industrial production simply and economically. More particularly, the method allows spinning and winding at high draw-off speeds of at least 2200 m/min and the production of yarn reels with a yarn weight higher than 2 kg, especially higher than 4 kg, wound yarn reels in the form of uniform packages Shaped, free of bumps and flaking strands.

→The use of spinning additives makes it possible to obtain draw-off speeds up to 6000m/min. As a result, the plant can be operated particularly economically.

→ Thus, the polyester multifilament yarns obtainable by the process can be further processed and used in large-scale industrial production simply and economically in operations of drawing or drawing texturing. In this operation, deformation can be carried out at speeds up to 450 m/min.

→ Due to the high uniformity of the polyester multifilament yarn obtainable from the process, a good package build can be easily obtained to ensure uniform and sufficiently defect-free dyeing and further processing of the polyester multifilament yarn.

→ The rolls obtained in winding are stable in shape and can be easily removed from the winding mandrel and retain their shape even after storage for up to e.g. 4 weeks or at temperatures up to 65 °C, especially at temperatures After transportation at a temperature between the glass transition temperature and 65°C.

→ Higher elongation at break and thus higher draw ratios in further processing are achieved at higher spinning speeds than without additives, favoring process economy.

→ The obtained POY desizing shrinkage of 0-10% ensures high stability of yarn parameters in storage. Even relatively high transport temperatures of up to 65°C only lead to a decrease in desizing shrinkage of no more than 10%. Deformation of the wound roll does not occur.

→ Yarns obtained by tensile texturing of multifilament yarns have high elongation at break and high tenacity at break.

The following part describes the invention in more detail with reference to the accompanying drawings, in which

Figure 1 is a schematic diagram of an apparatus for tensioning or winding one or more multifilaments,

Fig. 2 is a schematic diagram of a cheese-like yarn roll,

Figure 3 is a schematic illustration of a textured yarn roll characterized by stiff edges and a saddle shape in the waist-like center.

The present invention provides a production of polyester multifilament yarns containing not less than 85% by weight of polybutylene terephthalate and/or polytrimethylene terephthalate, based on the total weight of the monofilaments and winding methods. Polybutylene terephthalate (PBT) and/or polytrimethylene terephthalate (PTMT) are known to those skilled in the art. Polybutylene terephthalate (PBT) can be obtained by polycondensation of terephthalic acid and equimolar amount of 1,4-butanediol, and polybutylene terephthalate (PTMT) can be Obtained by polycondensation of terephthalic acid and equimolar amounts of 1,3-propanediol. Mixtures of the two polyesters can also be used. PTMT is preferred in the present invention.

The polymers may be homopolymers or copolymers. Useful copolymers include, in addition to recurring units of PTMT and/or PBT, recurring units of customary comonomers such as ethylene glycol, di Glycol, triethylene glycol, 1,4-cyclohexanedimethanol, polyethylene glycol, isophthalic acid and/or adipic acid. However, for the present invention polyester homopolymers are preferred.

The polyesters in the present invention may contain other additives such as catalysts, stabilizers, antistatic agents, antioxidants, flame retardants, dyes, dye absorption modifiers, light stabilizers, organic phosphites, Optical brighteners and delustering agents. Preferably the polyester contains 0 to 5% by weight of additives, based on the total weight of the monofilaments.

The polyesters may additionally contain small fractions, preferably up to 0.5% by weight, based on the total weight of the monofilaments, of branched constituents. In the present invention, preferred branched components are polyfunctional acids, such as trimellitic acid, or 1,2,4,5-pyrellitic acid, or tri- to hexavalent alcohols, such as trimethylolpropane, pentaerythritol, di Pentaerythritol, glycerol or the corresponding hydroxy acids.

In the present invention, PBT and/or PTMT is mixed with 0.05% to 2.5% by weight of an additive polymer as an extensibility enhancer based on the total weight of the monofilament. Additive polymers which are particularly useful for the present invention are the following polymers and/or copolymers:

1. The polymkeric substance that can obtain by polymerization of the monomer of general formula (I):

wherein R ¹ and R ² are substituents consisting of optional atoms C, H, O, S, P and halogen atoms, and the total molecular weight of R ¹ and R ² is at least 40. Examples of monomer units are acrylic acid, methacrylic acid and _CH2 =CR-COOR', where R is an H atom or a _CH3 group, and R' is a _C1-15 aryl group or a _C5-12 cycloalkyl group Group or C _6-14 aryl group, also styrene and C _1-3 alkyl substituted styrene.

2. Copolymers containing the following monomer units:

A = acrylic acid, methacrylic acid or CH ₂ =CR-COOR', where R is an H atom or a CH ₃ group, R' is a C _1-15 alkyl group or a C _5-12 cycloalkyl group or C _6-14 aryl groups,

B = styrene or C _1-3 alkyl substituted styrene,

The copolymer consists of 60 to 98% by weight of A and 2 to 40% by weight of B, preferably 83 to 98% by weight of A and 2 to 17% by weight of B and more preferably 90 to 98% by weight of A and 2 to 10% by weight % of B (100% by weight in total).

3. Copolymers containing the following monomer units:

C = styrene or C _1-3 alkyl substituted styrene,

D = one or more monomers of formula II, III or IV

Wherein R ³ , R ⁴ and R ⁵ are each an H atom or a C _1-15 alkyl group or a C _6-14 aryl group or a C _5-12 cycloalkyl group. The copolymer consists of 15 to 95% by weight of C and 2 to 80% by weight of D, preferably 50 to 90% by weight of C and 10 to 50% by weight of D and more preferably 70 to 85% by weight of C and 15 to 30% by weight Consists of D (total of C and D: 100% by weight) by weight.

4. Copolymers containing the following monomer units:

E = acrylic acid, methacrylic acid or CH ₂ =CR-COOR', where R is an H atom or a CH ₃ group, R' is a C _1-15 alkyl group or a C _5-12 cycloalkyl group or C _6-14 aryl groups,

F = styrene or C _1-3 alkyl substituted styrene,

G = one or more monomers of formula II, III or IV

wherein R ³ , R ⁴ and R ⁵ are each a H atom or a C _1-15 alkyl group or a C _5-12 cycloalkyl group or a C _6-14 aryl group;

H = one or more ethylenically unsaturated monomers, copolymerizable with E and/or with F and/or G, selected from alpha-methylstyrene, vinyl acetate, methacrylic acid different from E esters, acrylates, acrylonitrile, acrylamide, methacrylamide, vinyl chloride, vinylidene chloride, halogen-substituted styrenes, vinyl ethers, isopropenyl ethers and dienes,

The copolymer consists of 30 to 99% by weight of E, 0 to 50% by weight of F, >0 to 50% by weight of G and 0 to 50% by weight of H, preferably 45 to 97% by weight of E, 0 to 30% by weight % of F, 3 to 40% by weight of G and 0 to 30% by weight of H, and more preferably 60 to 94% by weight of E, 0 to 20% by weight of F, 6 to 30% by weight of G and 0 to 20% by weight Consists of H, (total of E, F, G, and H 100% by weight) by weight.

Ingredient H is an optional ingredient. Although the advantages mentioned in the present invention can already be obtained by copolymers containing components selected from E to G, the advantages to be obtained according to the present invention can also be obtained according to the present invention by using monomers selected from H in the construction of copolymers .

Component H is preferably chosen such that it does not adversely affect the properties of the copolymers used.

Component H can be used, inter alia, to modify the properties of the copolymer in a desired manner, for example by increasing or improving the fluidity when heated to the melting temperature, or to reduce any residual color in the copolymer or by using polyfunctional The monomers thus introduce some degree of crosslinking into the copolymer.

In addition to these purposes, H can also be selected in such a way that the copolymerization of any E to G components is increased or firstly as for MA and MMA which do not polymerize by themselves so that their copolymerization is possible upon addition of a third component such as styrene.

Monomers useful for this are vinyl esters, acrylates such as methyl acrylate and ethyl acrylate, methacrylates other than methyl methacrylate such as butyl methacrylate and ethylhexyl methacrylate Esters, acrylonitrile, acrylamide, methacrylamide, vinyl chloride, vinylidene chloride, styrene, α-methylstyrene and various halogen-substituted styrenes, vinyl ethers, isopropenyl ethers, dienes, e.g. 1,3-Butadiene and divinylbenzene. It is especially preferred to obtain a reduction in the color of the copolymer by using electron-rich monomers, for example by using vinyl ether, vinyl acetate, styrene or alpha-methylstyrene.

Among these compounds of component H, especially preferred are aromatic vinyl monomers such as styrene or α-methylstyrene.

The production of the above mentioned polymers and/or copolymers is well known to those skilled in the art. Details can be obtained, for example, from document WO 99/07927, the disclosure of which is hereby incorporated by reference in its entirety.

For the present invention it is especially preferred that the additive polymers and/or copolymers are in the form of bead polymers with a particle size in a particularly suitable range. The additive polymers and/or copolymers to be used according to the invention, for example by mixing them into the melt of the fiber polymer, are advantageously in the form of granules with an average diameter in the range of 0.1 to 1.0 mm. However, larger or smaller beads or pellets can also be used. The additive polymers and/or copolymers can also already be contained in the fragments of the matrix polymer so that no metered addition is required.

Also preferred are additive polymers and/or copolymers which are amorphous and insoluble in the polyester matrix. They preferably have a glass transition temperature of from 90 to 200° C., the glass transition temperature being determined by known methods, preferably by differential scanning calorimetry. Further details may be obtained from the prior art, for example from WO 99/07927, the disclosure of which is hereby incorporated by reference in its entirety.

Preferably the additive polymer and/or copolymer is selected such that the ratio of the viscosity of the additive polymer and/or copolymer melt to the viscosity of the matrix polymer is in the range of 0.8:1 to 10:1 and preferably in the range of 1.5:1 to 8:1 range. The viscosity of the melt is measured in a known manner using an oscillatory rheometer at an oscillation frequency of 2.4 Hz and a temperature equal to the melting point of the matrix polymer plus 28°C. For PTMT, the temperature for measuring melt viscosity is 255°C. Further details can still be found in WO 99/07927. The melt viscosity of the additive polymer and/or copolymer is preferably higher than the viscosity of the matrix polymer, and it has been confirmed that the selection of the intrinsic viscosity of the additive polymer and/or copolymer and the selection of the viscosity ratio have a great influence on the performance of the yarn product. contribute to optimization. Given an optimized viscosity ratio, it is possible to minimize the amount of additive polymer and/or copolymer used, thereby, inter alia, improving the economics of the process. Preferably the polymer mixture to be spun contains 0.05 to 2.5% by weight, more preferably 0.25 to 2.0% by weight of additive polymers and/or copolymers.

Selection of a suitable viscosity ratio provides a combination of a narrow particle size distribution of the additive polymer and/or copolymer in the polymer matrix and a desired fibrillar structure of the additive polymer and/or copolymer in the fibers. The higher glass transition temperature of the additive polymer and/or copolymer compared to the matrix polymer ensures rapid solidification of this fibril structure in the spun fibers. The maximum particle size of the additive polymer and/or copolymer emerging from the spinneret is about 1000 nm and the average particle size is 400 nm or less. The favorable fibrillar structure is obtained after the fibers have been drawn down, the monofilaments contain at least 60% by weight of additive polymers and/or copolymers, which are present in the form of fibrils with a length in the range of 0.5 to 20 μm and a diameter in the range of 0.01 to 0.5 μm.

The polyesters useful in the present invention are preferably thermoplastically formable polyesters that can be spun and wound. Particularly advantageous polyesters here have an intrinsic viscosity of from 0.70 dl/g to 0.95 dl/g.

Polymer melts can be obtained, for example, directly from the polycondensation plant or produced from solid polymer chips by a melt extruder.

One known method of metering spinning additives is to meter them into the matrix polymer in the molten or solid state and to disperse them therein to form fine particles. A device as described in DE 10022889 can advantageously be used.

The method of the invention is not limited to specific spinning methods; rather, all conventional spinning methods known from the prior art can be used. Therefore, although a particularly preferred spinning operation will be described below, reference should be made to the general technical knowledge, in particular to the disclosures in Synthetische Fasern, F. Fourné, Hanser, Munich, 1995.

In a particularly preferred embodiment of the method of the present invention, the polyester melt or melt mixture is pumped into the spinneret pack at a constant speed by a spinning pump, and the polyester melt or melt mixture passes through the die plate of the pack Mesopore extrusion to form molten filaments, the pumping speed will be calculated by a known equation to obtain the desired fiber linear density.

The melt can be prepared, for example, from polymer chips in an extruder, in which case it is particularly advantageous to first dry the chips to a water content of ≤30 ppm, in particular ≤15 ppm.

The temperature of the melt (often referred to as the spinning temperature and can be measured above the spinning pump) depends on the melting point of the polymer or polymer mixture used. Preferably the temperature is within the range given by Equation 1:

Formula 1:

T _m +15°C≤T _Sp ≤Tm+45°C

here

T _m is the melting point of polyester [°C]

T _Sp is the spinning temperature [°C].

The specified parameters serve to limit hydrolytic and/or thermoviscous degradation to a very low degree. In the present invention, it is desired that the viscous degradation is below 0.12 dl/g, especially below 0.08 dl/g.

The homogeneity of the melt has a direct influence on the material properties of the spun filaments. In addition to the static mixer in the production line, it is preferred to use another static mixer which has at least one element and is installed below the spinning pump to homogenize the melt.

The die plate temperature, which depends on the spinning temperature, is controlled by the plate's secondary heating system. Useful secondary heating systems include, for example, spinning boxes heated with "Difer heat exchangers" or additional convective or exothermic heaters. The die plate temperature is usually equal to the spinning temperature.

The temperature increase at the die plate can be achieved by the pressure gradient of the spinneret pack.

Known derivations, eg K. Riggert "Fortschritte in der Herstellung von Polyester-Reifenkordgarn" Chemiefasern, 21, p. 379 (1971) describe a temperature increase of about 4° C. per 100 bar pressure drop.

Another possibility to control the pressure of the port template is to use loose filter media, especially steel grit and/or filter discs with an average particle size between 0.10mm and 1.2mm, preferably between 0.12mm and 0.75mm, which can It is shaped into woven or non-woven metal fibers with a fineness of ≤40 μm.

Additionally, the pressure drop in the die plate holes contributes to the total pressure. The die plate pressure is preferably between 80 bar and 450 bar, especially between 100 bar and 250 bar.

Spinning thread elongation i _sp , i.e. the ratio of drawing speed to extrusion speed, can be calculated according to US 5250245 from the density of the polymer or polymer mixture, spinneret hole diameter and monofilament linear density by Equation 2:

Formula 2:

i _sp =2.25·10 ⁵ ·(δ·π)·D ² (cm)/dpf(den)

here

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

D = spinneret hole diameter [cm]

dpf = denier/monofilament [den].

For the invention, advantageously, the spun yarn elongation is between 70 and 500, in particular between 100 and 250.

The length/diameter ratio of the spinneret holes is preferably between 1.5 and 6, especially between 1.5 and 4.

The extruded monofilaments pass through a quench delay zone. The quench delay zone is arranged directly below the spinning pack as part of the recessed zone, in which the monofilaments coming out of the spinneret hole are protected from the direct action of the cooling gas and the spinning yarn is delayed Stretch or cool. The active part of the recessed area is built into the spin beam as an extension of the spin pack so that the filaments are surrounded by a thermal wall. The passive part consists of an insulating layer and an unheated frame. The length of the active recess is advantageously between 0 and 100 mm, while the length of the passive part is advantageously between 20 and 120 mm, preferably a total length of 30-200 mm, preferably 30-120 mm.

As an alternative to the active recess, a reheater can be arranged below the spin box. In contrast to the actively recessed area, this area of cylindrical or rectangular cross-section then contains at least one heating system which is independent of the spinning beam.

For quenching systems with radial holes concentrically surrounding the yarn, a cylindrical shield can be used to obtain a quenching delay.

The monofilaments are then cooled below the solidification temperature. For the purposes of this invention, solidification temperature refers to the temperature at which a melt transforms into a solid state.

In the present invention it has been determined to be particularly advantageous to cool the filaments to a temperature at which they are substantially non-stick. In particular it is particularly advantageous to cool the monofilaments below their crystallization temperature, in particular below their glass transition temperature.

Technical means for quenching or cooling of monofilaments are available from the prior art. According to the invention, it is particularly useful to use cooling gas, especially cold air. The temperature of the cooling air is preferably in the range of 12°C to 35°C, especially in the range of 16°C to 26°C. The speed of the cooling air is advantageously between 0.20m/s and 0.55m/s.

The monofilaments may be cooled using a single ended system such as a single cold tube comprising a perforated wall. Cooling of each monofilament can be achieved by active cooling air supply or by self-priming of the filaments. As an alternative to separate tubes, it is also possible to use the familiar cross-flow quenching system.

In a particular embodiment of the cooling and yarn elongation zone, the monofilaments emerging from the delay zone are exposed to cool air in a zone with a length of 10 to 175 cm and preferably 10-80 cm. A zone with a length of 10-40 cm is particularly suitable for monofilaments with a linear density ≤ 1.5 dtex/filament when taken up, and a zone with a length of 20-80 cm is particularly suitable for monofilaments with a linear density between 1.5 and 9.0 dtex/filament . The monofilament and the accompanying air are then passed together through a channel of reduced cross-sectional area by controlling the shrinkage of the cross-sectional area and the dimension in the direction of spinning yarn transport, wherein the ratio of air speed to spinning line speed at draw-off is between 0.2 and 20:1, preferably in the range of 0.4 to 5:1.

After the monofilaments have cooled to a temperature below the solidification point, they are gathered together to form a yarn bundle. According to the invention, a suitable distance from the converging point to the lower surface of the spinneret can be determined by conventional methods using online measurement of yarn speed and/or yarn temperature, for example using TSI/German Laser Doppler Wind Velocity Meter or Goratec/Germany model is IRRIS 160 infrared camera measurement. A range from 500 to 2500 mm, preferably from 500 to 1800 mm is advantageous. Monofilaments obtained from spinning with a linear density ≤ 3.5 dtex are preferably gathered into a multifilament bundle over shorter distances ≤ 1500 mm, while thicker filaments are preferably gathered over longer distances.

For the present invention it is advantageous that all surfaces which are to be in contact with the spun yarns consist of a particularly low-friction material. This substantially avoids yarn breakage and provides a higher quality yarn. Particularly suitable for the purpose of the present invention are low-friction surfaces of the Ceramtec/Germany "Tribofil" specification.

The filaments are funneled to oiling needles that provide spinning oil to the yarn at a uniform speed. A particularly suitable grease needle is characterized by an inlet part, a yarn tube with a grease hole and an outlet part. The inlet section resembles a funnel, thus avoiding dry contact of the monofilaments. The contact point of the monofilaments takes place in the yarn tube after the end of the supply of yarn oil. The width of the yarn tube and the oil inlet hole should be adapted to the linear density of the yarn and the number of monofilaments. Holes and widths of 1.0 mm to 4.0 mm are particularly suitable. The outlet portion of the oil needle is configured to preferably contain a homogenized area of the oil pool. Such oilers are available eg from Ceramtec/Germany or Goulston/USA.

The uniformity of oil application is very important to the present invention. The homogeneity can be determined, for example, with a Rossa meter according to the method described in Chemiefasern/Texttilindustrie, 42/94 (November 1992) p. 896. Preferably, such a process provides a standard deviation value of no more than 90 digits, especially less than 60 digits. For the present invention, it is particularly preferred to use standard deviation values for oils of less than 45 figures, especially less than 30 figures. A standard deviation value of 90 or 45 figures corresponds approximately to a coefficient of variation of 6.2% or 3.1%, respectively.

For the present invention it is especially beneficial to design the post spinning line and pumps so that they can be automatically vented to avoid air bubbles which can cause significant variations in oil application.

According to the invention it is particularly preferred to wind the monofilaments before the yarn is wound. In the present invention, nozzles with closed yarn tubes are particularly suitable, since such a system prevents the yarn from stopping in the feed opening, even at low yarn tensions and high air pressures. The winding nozzles are preferably arranged between the godets, and the outlet tension of the yarn is controlled by different speeds of the inlet and outlet godets. The exit tension of the yarn should not exceed 0.20cN/dtex, and should mainly be between 0.05cN/dtex and 0.15cN/dtex. Winding air pressure is between 0.5 and 5.5 bar, or up to 3.0 bar for takeup speeds up to 3500 m/min.

The yarn is preferably wound to a node count of at least 10 n/m. The largest nodeless gap is less than 100 cm, and it is especially interesting that the node number coefficient variation value is less than 100%. Advantageously, the air pressure used is higher than 1.0 bar to provide a knot number > 15n/m, which is manifested by a high uniformity, since the coefficient of variation does not exceed 70% and the maximum knot-free gap is 50 cm. In practice, the LD type system from Temco/Germany, the dual system from Slack & Parr/USA or the Polyjet from Heberlein have been found to be particularly useful.

The peripheral speed of the first godet unit is considered to be the draw-off speed. Additionally godet systems can be used in winding equipment to form coils (spindles) on tubes for drawing, thermosetting and/or relaxing of multifilaments before the yarn is wound.

In a particularly preferred embodiment of the invention, the multifilament is heat-treated before it is wound, preferably at a temperature in the range from 50 to 150° C., by virtually any known method. It has been determined that the use of heated godets will be most beneficial for polyester multifilament yarns that require heat treatment. Godets useful with the present invention include those generally described in Fourné, Synthetische Fasern, Hanser, Munich (1995).

In another preferred embodiment of the invention, the polyester multifilament yarn is thermally treated with hot gas, especially with hot air.

In a third preferred embodiment of the present invention, radiant heating is used to heat treat the polyester yarn multifilaments.

The heat treatment of multifilaments can also be obtained by introducing the yarns to an elongated heating surface in close proximity but substantially out of contact with the heating surface, in this case suitable embodiments of this method are described for example in document EP 731196 in.

A stable, defect-free coil is an essential prerequisite for defect-free yarn winding and for ideally defect-free further processing. Therefore, in the present invention it has been found most advantageous to use a winding tension in the range of 0.025 cN/dtex - 0.15 cN/dtex, preferably in the range of 0.03 cN/dtex - 0.08 cN/dtex.

Another important parameter in the method of the invention is the setting of the yarn tension set on or between the drawing guides. As will be known, this tension is basically composed of the Hamana actual orientation tension, the frictional tension created by the yarn guide and oiler, and the yarn-air frictional tension. For the present invention, the yarn tension over and between the drawing wire discs is in the range of 0.05 cN/dtex to 0.20 cN/dtex, and preferably in the range of 0.08 cN/dtex to 0.15 cN/dtex.

Too low a tension of less than 0.05 cN/dtex will not provide the desired degree of partial orientation. When the tension exceeds 0.20 Cn/dtex, this tension will frequently cause a memory effect during winding and storage of the spindle, and it will lead to deterioration of yarn parameters.

According to the invention, the tension is controlled by the distance from the spinneret to the lubricator, the frictional surfaces and the length of the gap between the lubricator and the drawing wire reel. This length preferably does not exceed 6.0 m, and preferably does not exceed 2.0 m, the spinning system and the drawing machine being arranged in a parallel configuration to ensure a straight yarn path.

The geometric parameters also describe the conditioning time to the yarn between the collection point and the winding point. Rapid relaxation during this period can affect the quality of the yarn roll formation. The conditioning time thus defined is preferably between 50 and 200 ms.

According to the present invention, the winding speed of POY is preferably between 2200 m/min and 6000 m/min. It will be advantageous to choose a speed between 2500m/min and 6000m/min. For polymer mixtures, winding at speeds in the range from 3500 m/min to 6000 m/min is especially preferred.

In the present invention, the coiled polyester multifilament yarn is heat treated at a temperature ranging from >45°C to 65°C. The duration of the heat treatment can be chosen freely; however, this time is of course significantly longer than is the case with known monofilament treatment methods using methods such as godets or hot rails. According to the invention, it has been found that it is most advantageous to heat-treat the coiled yarn rolls in the above-mentioned temperature range for at least 5 minutes, preferably at least 10 minutes, more preferably 20 minutes, especially at least 30 minutes, The times mentioned are counted from the start of the winding operation.

Heat treatment may be carried out in any known manner, suitable methods including those in which the principle of heat treatment is based on heat conduction, heat convection and/or heat radiation. In a preferred embodiment of the invention, the wound yarn roll is thermally treated by using heated rolls or rollers, preferably by using at least one contact roller which allows simultaneous measurement and control of the winding speed. In another preferred embodiment of the present invention, radiant heating is used to heat treat the coiled yarn.

In a third preferred embodiment of the invention, the wound package of yarn is heat treated with hot gas. Suitable gases are air and inert gases such as nitrogen, helium and/or argon. In this context, the use of hot air has been determined to be most advantageous. The temperature of the hot gas is preferably uniform so as to ensure that the temperature in the shell is in the range of greater than 45°C to 65°C. The temperature of the hot gas is thus preferably in the range of greater than 45°C to 65°C. The relative humidity of the gas is preferably from 40 to 90%. The gas flow rate at the inlet is preferably 5 to 100 m ³ /h.

The heat treatment of wound yarn reels is preferably accomplished using an apparatus for winding one or more multifilament yarns, comprising a shell and a rotatable spindle on which a tube can be securely mounted so that the tube is loaded into the shell. The heat treatment is preferably accomplished in the shell, preferably by heating the wound roll of yarn by heat conduction, heat convection and/or heat radiation.

At this point, the spindle that can rotate is part of the winder. At least one tube is clamped to the chuck of the rotatable spindle, and at least one multifilament yarn is wound onto the at least one tube to form at least one wound yarn package. After winding, at least one tube with the wound yarn package can be removed from the chuck.

Any type of winder known from the prior art can be used in the present invention as long as the purpose of the present invention can be achieved. For further details reference is made to the technical literature, in particular to Synthetische Fasern by F. Fourné, Hanser, Munich (1995). As with conventional, prior art winders, the invention allows one or more multifilaments, in particular 1 to 12, to be wound simultaneously on one spindle. According to the present invention, in order to increase the efficiency of the spinning operation, it is especially preferred that many multifilaments are wound simultaneously.

The housing of the device for winding one or more multifilament yarns can be made of any known material. However, it has been found to be particularly advantageous for the shell to be made of a thermally insulating material, preferably a soundproof material. Suitable materials include plastics, especially plastics with a glass transition temperature greater than 65°C, metals such as stainless steel and metal alloys. The heat insulating material may have a single layer or a multilayer structure of two, three or more layers. The thermal conductivity of the insulating material is preferably less than 10 W/(m·k), more preferably less than 1 W/(m·k), even more preferably less than 0.5 W/(m·k) and most preferably less than 0.1 W/(m·k) . When the thermal and preferably sound insulating material is a three-layer structure, wherein the middle layer consists of a thermally insulating material with a thermal conductivity of less than 0.1 W/(m·k) and the outer layer preferably contains and advantageously consists of a metal or a metal alloy Particularly favorable results are obtained.

The housing is preferably sized to completely accommodate the winder or at least the chuck with the largest diameter tube comprising the coil of yarn being wound. It has also been determined that it is advantageous for any additional winding devices, preferably containing contact rollers for controlling the winding speed and preferably traversing devices, to be also contained in the housing. This minimum size of the shell allows a defect-free winding operation of high quality yarn.

As an option, it is also advantageous to minimize the size of the shell in order to make it possible to obtain standard working conditions outside the shell in the winding room and to minimize the expense of heating the space inside the shell. The shell should be preferred to enable the introduction of multifilament yarns in a simple manner, the easy removal of wound yarn reels and the production of wound yarn reels with a high weight, preferably more than 2 kg and more preferably 4 kg.

In a particularly preferred embodiment of the invention, the heat treatment of the wound yarn reel is achieved by means of at least one hot gas inside the shell, preferably by introducing the gas into the shell through an inlet and from it, preferably through an outlet. Remove from the shell. It has been found to be particularly advantageous to interconnect the inlet and the outlet so that the gas can then circulate in the circulation system comprising the inlet and the outlet. With reference to the direction of movement of the yarn, it is advantageous for the gas to enter from the rear of the tube and exit from the front of the tube. While the gas can also be heated inside the shell, it is preferred to heat it outside the shell to ensure a stable and consistent temperature scale within the shell.

In this embodiment, it is particularly advantageous that the temperature to be measured inside the shell is measured by means of at least one temperature sensor and that the temperature of the gas is brought into line with it by suitable heating, preferably outside the shell, so that the shell The temperature within drops to greater than the range of 45°C to 65°C. Here, it is preferable to connect the temperature sensor to the heating unit for heating the gas, so that the temperature of the gas can be controlled within a predetermined range, preferably greater than 45°C to 65°C.

The temperature is measured inside the shell, compared with a predetermined value and depending on the temperature difference the temperature of the heating gas is adjusted accordingly (raised, lowered or maintained) so that the temperature inside the shell falls within the required range favorable.

Furthermore, it is advantageous to measure the temperature inside the shell at at least two points, preferably in front and behind the sleeve, with reference to the direction of movement of the yarn, to check and ensure that the temperature inside the shell is constant. Temperature gradients are avoided by suitable temperature configuration of the gas and/or its flow rate.

In order to introduce the multifilaments before the start of winding, the shell preferably has an opening, and particularly preferably the opening is in the form of an elongated hole. Viewed from the running direction of the yarn, the open long holes are preferably arranged so that the multifilament yarn can be introduced laterally. During the winding process, it is advantageous for the elongated hole to be partly covered by suitable means, so that the interior of the shell is sealed off from its surroundings, so that possible temperature gradients within the shell can ideally be avoided. In a particularly preferred embodiment of the invention, the cover is in the form of a flap, which protects the outer surface of the shell, which covers the slotted part during the spinning and winding operations, and which, when the multifilament yarn is introduced, It can be turned on again when it is online. Preferably the flap has one or more slits through which the multifilament yarn can enter the shell when the flap is closed. The location and size of the one or more openings are appropriately selected according to the transverse length of the wound yarn roll.

The winding apparatus which may be used in this embodiment preferably contains a traversing device for controlling the specific shape of the wound yarn roll. The use of a specific traversing device is not limited in the present invention; rather, any known traversing device can be used as long as the object of the present invention is achieved.

In this embodiment of the invention, the position of the traversing device is not subject to any restrictions; for example, it may be arranged outside the shell, preferably directly above the opening for introducing the multifilament yarn into the shell, at the In this case, the opening is preferably in the form of an elongated hole, which can be covered by a flap with one or more slits. The slots preferably run parallel to the tube. According to the horizontal length, select the corresponding length of the slot long hole.

Nevertheless, the traversing device is preferably arranged in the housing, preferably before the tube onto which the multifilament yarn is wound, with reference to the direction of movement of the yarn. This makes it possible to minimize the size of the openings, so that the occurrence of temperature gradients within the shell is ideally suppressed. In this case, too, the opening is preferably in the form of an elongated hole and can be covered by a flap with one or more slits, the elongated hole preferably extending parallel to the tube.

According to the invention, in order to remove the wound yarn reel from the device, this device can be opened in a suitable manner, in this case, for this opening, provided during the spinning and winding process An opening that can be closed to ensure a constant temperature inside the shell. A particularly preferred embodiment of the closable opening is a door that can be opened to introduce multifilament yarn or remove the resulting wound yarn roll, and during spinning and winding, the door can be closed. close. The closable opening is preferably arranged on the front side of the housing. Opening the door for three periods of time to remove the wound roll during the automatic change of the mandrel in the winding position has been determined not to be critical.

Figure 1 is a schematic diagram of a particularly suitable embodiment of the apparatus. The winding device 2 has a housing 4 . In the illustrated embodiment, the shell 4 has a lower wall 6, an upper wall 8, two side walls 10, 12, a front wall 14 and a rear wall 16, the upper wall 8 facing the incoming multifilament yarn. direction. The front wall has the function of a door, ie the housing 4 can be opened or closed through the front wall 14 . At the rear wall 16 a drive unit 18 is provided outside the housing 4 .

The upper wall 8 has an elongated opening 20 which extends from the front wall 14 in parallel to the side walls 10 , 12 in the direction of the rear wall 16 . The opening 20 is partially covered by a flap 22 comprising a slit 24 through which a multifilament yarn 26 can pass through the opening 20 into the shell 4 . Since the opening 20 extends as far as the front wall 14, the multifilament yarn 26 can be introduced from the side of the shell 4 when the front wall 14 and the flap 22 are opened.

Referring to the direction of movement of the multifilament yarn 26 , indicated by arrow A in FIG. 1 , the traversing unit 28 is arranged behind the opening 20 in the housing 4 . The traversing unit is connected to and driven by a drive unit 18 on the rear wall 16 . Referring to direction A of movement from the multifilament yarn 26 , for example, four tubes 30 have been clamped onto the chucks of the rotatable spindles arranged behind the traversing unit 28 , in the housing 4 . The spindle is connected to the drive unit 18 such that during operation of the drive unit 18 the spindle and the tube 30 clamped to the spindle can rotate about their axis.

Two temperature sensors 32 are arranged in the shell 4 for measuring the temperature inside the shell and controlling the heat flux, one sensor 32 is arranged behind the tube 30 and the other sensor is in front of the tube 30, referring to the multifilament yarn Direction A of movement of wire 26 .

The housing 4 additionally contains an outlet 34 arranged on the upper wall 8 and an inlet 36 arranged on the rear wall 16 . In other words, the outlet 34 is arranged before the tube 30 and the inlet 36 after the tube 30 with reference to the direction of movement A from the multifilament yarn 26 . The outlet 34 can optionally be connected to a heating and blowing unit 38 via a circulation system 40, shown in dashed lines in Figure 1, so that the heated gas can be circulated and process costs minimized. The inlet 36 is connected to the heating and blowing unit 38 through a circulation system 42 . The heating and blowing unit 38 heats gas, such as air, and blows it in the direction of arrow B in FIG. 1 so that the gas is circulated through the shell 4 . By controlling the setting of the parameters of the heating and blowing unit 38, with reference to the values measured by the sensor 32, it is possible to control the temperature in the area where the pipes are arranged.

The operation of the above-mentioned device 2 will now be described. First, the multifilament yarn 26 has to be fixed (preferably by means of a pneumatic yarn suction gun) on the tube clamped on the chuck 30 . For this reason, the front wall 14 and the flap 22 must be opened so that the multifilament yarn 26 can be introduced into the slot-shaped opening 20 . After the multifilament yarn 26 is introduced into the opening 20, the piecing operation is started by the winder control system, and the front wall 14 and the flap 22 can be closed again so that each multifilament yarn can only Through its own slit 24 in the flap. The yarn wound onto the tube 30 is traversed to construct the wound yarn package 44 . During winding of the multifilament yarn 26 , hot gas enters the shell 4 through the inlet 36 to heat the shell and the wound yarn roll 44 on the tube 30 . The hot gas enters the heating and blowing unit 38 via the outlet 34 in order to obtain there a preselected temperature for winding the yarn package 44 and the multifilament yarn 26 .

The method of the invention makes it possible to produce on the tube 30 a package-like wound yarn reel 44 as shown in FIG. 2 . Shrinkage and deformation of the wound yarn roll 44 during storage will either prevent the wound yarn roll from being removed from the chuck or form a saddle 50 with a hard edge 52 (as shown in FIG. 3 ). that) will no longer be observed. Unwinding problems will thus no longer occur during the further processing of the wound yarn reel. The wound polyester yarn rolls obtainable by the present method exhibit improved long-term stability during storage and are insensitive to high temperatures during storage and transport. More particularly, they retain their beneficial properties and their cheese-like shape even in prolonged storage, eg 4 weeks.

Under standard conditions, after a storage period of 4 weeks, the polyester multifilament yarn obtainable according to the present invention

a) the elongation at break is between greater than 60% and 165%, preferably between 75% and 145%,

b) Desizing shrinkage rate is 0 to 10%,

c) The nominal Uster (normal Uster) is lower than 1.1%, preferably ≤0.9%,

d) change in breaking load factor ≤ 4.5%, and

e) Coefficient of variation of elongation at break ≤ 4.5%.

The term "standard conditions" is known to the person skilled in the art and is defined in German standard DIN53802. According to the standard conditions specified in DIN 53802, the temperature is 20±2°C and the relative humidity is 65±2%.

It is also particularly advantageous for the present invention if the desizing shrinkage measured directly after winding is between 0 and 10%, and after 4 weeks of storage under standard conditions it is lower than not more than 2% absolute. Shipping conditions of up to 65°C naturally lead to a further reduction in desizing shrinkage up to 10% absolute. Surprisingly, it has been established that POY spindles produced by this method have excellent further processing properties, it is possible to use higher draw ratios and draft Or stretch-textured yarns have high strength and uniform dyeability. For high residence times and relatively low temperatures considerably higher than those using only monofilament processing methods such as godets or hot rails, in POY positive elongation and low desizing shrinkage can only be achieved by heat treatment itself. invented method.

Methods for determining indicator material parameters are well known to those skilled in the art. They can be obtained from the technical literature. While most parameters can be determined by various methods, the following methods for determining silk parameters have proven particularly beneficial for the present invention:

The intrinsic viscosity is measured in an Ubbelohde capillary viscometer at 25°C and calculated by the familiar formula. The solvent used was a 3:2 w/w mixture of phenol and 1,2-dichlorobenzene. The concentration of the solution was 0.5 g of polyester per 100 ml of solution.

Melting point, crystallization temperature and glass transition temperature were each determined separately with a Mettler DSC calorimeter. The sample was first heated to 280°C to melt it and then quenched. DSC measurements were performed at a temperature range from 20°C to 280°C at a heating rate of 10K/min. The temperature is determined by the processor.

The multifilament density was determined in a density gradient column at 23±0.1°C. The reagents used are n-heptane (C ₇ H ₁₆ ) and carbon tetrachloride (CCl ₄ ). The obtained measurement results can be used to calculate the degree of crystallinity based on the density D _a of the amorphous polyester and the density D _k of the crystalline polyester. Calculation methods are described in the literature, eg for PTMT the corresponding values are D _a =1.295 cm ³ and D _k =1.429 cm ³ .

The linear density is determined in a known manner using a precision reel and weighing equipment. For POY, the pretension used is 0.05cN/dtex, and for DTY, it is 0.2cN/dtex.

In a Statimat device, the breaking strength and breaking elongation are determined under the following conditions: clamping length is 200 mm for POY and 500 mm for DTY, elongation is 2000 mm/min for POY and 1500 mm/min for DTY, The pretension is 0.05cN/dtex for POY and 0.2cN/dtex for DTY. The maximum breaking load value divided by the linear density is used to determine the breaking strength, and the breaking elongation is determined at the maximum load.

The desizing shrinkage rate is determined by treating the monofilament bundle in water at a temperature of 95±1°C for 10±1min under a tension-free state. The length of the monofilament bundle before and after heat treatment was measured at 0.2 cN/dtex by coiling up the monofilament bundle at a pretension of 0.05 cN/dtex (for POY) and 0.2 cN/dtex (for DTY). The desizing shrinkage is calculated in a known manner from the difference in lengths.

The crimp parameter of textured filaments can be measured according to DIN 53840 part 1 at an unwinding temperature of 120°C using a Texturmat instrument from Stein/Germany.

Nominal Uster values are measured using a 4-CX Uster Tester and results are given as Uster % values. The test speed is 100m/min, and the test time is 2.5min.

By virtue of the addition of the elongation enhancing additive at higher spinning speeds than without the additive, the theoretically calculated maximum draw ratios (Examples 1-3) can be obtained, which constitutes a productivity advantage in economic terms. The theoretically calculated maximum draw ratio is between 1.6 and 2.65, preferably between 1.75 and 2.45.

According to the invention, the further processing of the polyester multifilaments is simple, in particular stretch texturing. In the present invention, tensile deformation is preferably achieved at a deformation speed of at least 500 m/min, more preferably at a deformation speed of at least 700 m/min. The draw ratio is preferably at least 1.35:1, more preferably at least 1.40:1. It is particularly advantageous to carry out stretch texturing on a machine of the type with high temperature heaters, for example on the AFK machine from Barmag.

Fluffy monofilaments produced in this way exhibit a low number of defects and are dyed with disperse dyes without a carrier at the boil, giving excellent shade and uniformity.

The fluffy SET filaments produced according to the invention preferably have a breaking strength greater than 20 cN/tex and an elongation at break greater than 32%. In the case of bulky HE filaments (which can be obtained without heat treatment in the second heater), it is preferred to have a breaking strength of more than 20 cN/tex and a breaking elongation of more than 30%.

The bulk and elastic behavior of the multifilaments according to the invention is excellent.

The invention will now be described in more particular detail by way of illustrative embodiments of the invention, but the invention is not limited to these examples.

Invention Embodiments 1 to 3

spinning and winding

PTMT fragments with an intrinsic viscosity of 0.93dl/g, a melt viscosity of 325Pa s (measured at 2.4Hz and 255°C), a melting point of 227°C, a crystallization temperature of 72°C and a glass transition temperature of 45°C at 130°C Tumble dried to a moisture content of 11 ppm.

The chips were melted in a Barmag 3E4 extruder with a melt temperature of 255°C. Various amounts of Plexiglas 7N polymethyl methacrylate from Röhm GmbH/Germany, which had been previously dried to a residual moisture content of less than 0.1%, were added to the melt as elongation enhancers.

For this purpose, the polymer additives are melted in a melt extruder, fed by a gear metering pump to the feed device and from there inserted through injection nozzles onto the stream in the direction of the polyester component. The two melts were homogenized and finely dispersed in a Sulzer SMX static mixer with 15 processing units and an internal diameter of 15 mm.

The melt viscosity of Plexiglas 7N is 810Pa s (2.4Hz, 255°C), as a result, the viscosity ratio of additives and polyester melt is 2.5:1.

The amount of melt transported was 63 g/min with a residence time of 6 min, the amount metered from the spinning pump to the spinneret pack adjusted so that the linear density of POY was about 102 dtex. Various winding speed settings can be used. A unit of Fluitec's 10mm internal diameter static mixer type HD-CSE has been installed below the spinning pump, but above the access point into the spinneret pack. The secondary heating system for the production line and the spinning section (including pumps and spinneret packs) has been set to 255°C. The spinneret assembly contains 30mm high 350-500μm steel grit, also can be 20μm non-woven filter and 40μm textile filter as filter media. The melt was extruded from an 80 mm diameter spinneret plate containing 34 holes of 0.25 mm diameter and 1.0 mm in length. Die pressure is about 120-140bar.

The quench delay zone was 100mm long and consisted of a 30mm thick heated wall and a 70mm thick insulated and unheated frame. Air blown horizontally and counterclockwise across the spun yarn quenched the molten multifilaments along a length of 1500 mm. The air velocity for quenching is 0.35m/s, the temperature is 18°C, and the relative humidity is 80%. The filaments start to solidify about 800 mm below the spinneret.

Before pooling, a yarn oiler located at a distance of 1050 mm from the spinneret was used to provide spinning oil. The oiler has a TriboFil surface and a 1 mm diameter inlet. The amount of spin finish used was 0.40%, based on the weight of the fibers.

The collected yarn is then supplied to the winder. The distance from the oiler to the first takeoff godet is 3.2m. The conditioning time is between 95 and 140ms. A pair of godets are surrounded by the yarn in an S shape. Located between the godets is a Temco winding nozzle, which uses 1.5bar air to operate. Adapted to the speed setting, the winding speed of the Barmag SW6 winding machine is set at a winding yarn tension of about 6 cN. The winder is mounted in a box into which air is fed from the air heater by means of a blower, the process being closed loop controlled to establish a range of 63 cm around the rotating yarn reel inside the box approximately 20 cm. Temperature within ±1.5°C.

All additive levels lead to significant increases in production capacity. 10kg produced spindles can be easily removed from the winding mandrel. After 4 weeks of storage under standard conditions as defined in DIN 53802, the obtained POY yarns also retain a very good time constancy of the silk properties. The desizing shrinkage just after spinning and winding ranged from 5 to 8% and was no more than 2% abs. higher than the stored spindle. The deformability and dyeing uniformity obtained are excellent. The maximum draw ratio used was surprisingly high for the POY speeds used. For the maximum stretch ratio (DR) used subsequently, we can find its definition in EPS 0 080 274 page 6, line 51: DR = (1+POY elongation (%)/100). To simulate transport, the ingots with these parameters were exposed for 20 h in a heating chamber at a temperature of 60 °C. The shape of the spindle and the fabric data change only insignificantly.

Comparative Example 4

Invention Example 1 was repeated with the following difference: The additive metering system was separated from the production line so that no extensibility enhancer was added. In addition, the winder box was removed and a temperature of 34°C was established at the same measuring point around the wound roll at a room temperature of 24°C.

The absence of extensibility enhancer results in lower elongation compared to Inventive Example 1, resulting in a lower maximum DR. Correspondingly, the spinning capacity and thus its economy are also reduced. Insufficient heat treatment of the wound yarn resulted in a desizing shrinkage of about 53%, which decreased by about 9% abs. to 44% after storage. Subsequent heat treatment at 60°C as described above reduces the desizing shrinkage by about 40% abs.

Other parameters and specific data are summarized in Tables 1 to 4.

Table 1: Test parameters Test parameters Invention Example 1 Invention Example 2 Additive concentration [%] 0.7 1.0 Traction speed [m/min] 3520 4022 Winding speed [m/min] 3500 4000 Yarn elongation 182 181 silk tension Above Godet 1 [cN] 15.5 16 Between godets 1 max [cN] 13 12.5 Above Godet 2 [cN/dtex] 0.15 0.16 Between godets 2 max [cN/dtex] 0.13 0.12 Tension of wound yarn 1 [cN] 5.9 6.4 Tension of wound yarn2 [cN/dtex] 0.058 0.062 Winding box have have

¹ : absolute

² : Based on linear density

Table 1: Test parameters (continued) Test parameters Invention Example 3 Comparative Example 4 Additive concentration [%] 0.5 0 Traction speed [m/min] 4517 3520 Winding speed [m/min] 4455 3500 Yarn elongation 182 182 silk tension Above Godet 1 [cN] 19 15 Between godets 1 max [cN] 13 13 Above Godet 2 [cN/dtex] 0.19 0.15 Between godets 2 max [cN/dtex] 0.13 0.13 Tension of wound wire 1 [cN] 6.5 5.9 Tension of coiled wire2 [cN/dtex] 0.064 0.058 Winding box have none

¹ : absolute

² : Based on linear density

Table 2: Material properties of partially oriented PTMT monofilament ¹ Material properties Invention Example 1 Invention Example 2 Linear Density [dtex] 102.5 103 Breaking strength [cN/tex] 21.8 22.3 Elongation at break [%] 115.4 98.2 Nominal Uster [%] 0.90 0.84 Desizing shrinkage [%] 4.1 4.9 Breaking load CV [%] 2.5 3.1 Elongation at break CV [%] 2.9 3.3 Calculated maximum DR 2.15 1.98

CV: coefficient of variation

¹ : Measured after storage for 4 weeks under standard conditions

Table 2: Material properties of partially oriented PTMT monofilament ¹ Material properties Invention Example 3 Comparative Example 4 Linear Density [dtex] 102 102.5 Breaking strength [cN/tex] 23.1 25.6 Elongation at break [%] 79.1 79.1 Nominal Uster [%] 0.90 0.98 Desizing shrinkage [%] 6.4 44 Breaking load CV [%] 2.5 3.4 Elongation at break CV [%] 3.4 4.9 Calculated maximum DR 1.79 1.79

CV: coefficient of variation

¹ : Measured after storage for 4 weeks under standard conditions

Stretch deformation

The PTMT monofilament spindles of Inventive Examples 1 and 2 were stored for 4 weeks under standard conditions as defined in German Standard DIN 53802 and then sent to Barmag's FK6-S-900 stretch texturing machine to produce stretched SET monofilaments. The deformation test parameters are summarized in Table 3 and the material properties of the resulting bulky SET monofilaments are summarized in Table 4.

Deformation defects were determined using Barmag's UNITENS system at the following limit settings: UP/LP = 3.0 cN, UM/LM = 6.0 cN.

Table 3: Test parameters for tensile deformation Test parameters Invention Example 1 Invention Example 2 Speed [m/min] 700 700 stretch ratio 1.60:1 1.44:1 D/Y ratio 2.1 2.1 Heater 1 temperature [°C] 155 155 Heater 2 temperature [°C] 160 160 Deformation defects [n/10km] 0 0 yarn tension F1, above component [cN] twenty three twenty two F2, above component [cN] twenty one 20 F2-CV [%] 1.2 1.4

F ² -CV: Coefficient of variation of F ²

Table 4: Material properties of stretch-textured monofilaments Test parameters Invention Example 1 Invention Example 2 Linear Density [dtex] 69 79 Breaking strength [cN/tex] 25.3 23.8 Elongation at break [%] 34.8 35.3 Dyeability check uniform uniform

Claims (25)

1. be used to produce method with winding part oriented polyester polyfilament yarn, gross weight based on polyfilament yarn, described polyfilament yarn contains polybutylene terephthalate (PBT) (PBT) and/or the poly terephthalic acid-1 that is not less than 85 weight %, ammediol ester (PTMT), gross weight based on polyfilament yarn, contain at least a polymer extensibility reinforcing agent as additive of 0.05 weight % to 2.5 weight %, described method comprise by the polyester multifilament yarn of reeling involved in under in temperature range greater than 45 ℃ to 65 ℃ capable heat treatment provide can steady in a long-termly store and to store and transportation the reel for yarn of temperature-insensitive coiling of rising.

2. the process of claim 1 wherein that the reel for yarn of reeling is to heat-treat by the roller or the roller of heat.

3. claim 1 or 2 method wherein use radiant heat that the reel for yarn of reeling is heat-treated.

4. the process of claim 1 wherein and use hot gas that the reel for yarn of reeling is heat-treated.

5. the process of claim 1 wherein and the reel for yarn of reeling is heat-treated in the shell around one is centered around the pipe that supports the coiling reel for yarn.

6. the method for claim 5, wherein gas enters in the shell by inlet.

7. the method for claim 6, wherein gas leaves in shell by outlet.

8. the method for claim 7, wherein gas circulates in the circulatory system that comprises import and outlet.

9. the method for claim 7, wherein, the moving direction of reference yarn, gas enters from the pipe back and leaves from the pipe front.

10. the method for claim 8, wherein, the moving direction of reference yarn, gas enters from the pipe back and leaves from the pipe front.

11. the method for claim 6 is wherein at shell externally heating gas.

12. the method for claim 11 is wherein measured the temperature in the shell and is kept the gas temperature unanimity by suitable heating, thus make temperature in the shell be in＞45 ℃ to 65 ℃ scope in.

13. the process of claim 1 wherein that the coiling reel for yarn is to be cheese-form.

14. any one method in the above claim was wherein heat-treated under 50 ℃ to 150 ℃ temperature before reeling at least a polyester multifilament yarn.

15. the method for claim 14 is wherein heat-treated by using heatable draw-off godet at least a polyester multifilament yarn.

16. the method for claim 14 is wherein heat-treated by using hot gas at least a polyester multifilament yarn.

17. the method for claim 15 is wherein heat-treated by using hot gas at least a polyester multifilament yarn.

18. any one method in the claim 14 to 17 is wherein heat-treated by using radiant heat at least a polyester multifilament yarn.

19. the method for claim 1, this method comprises

A) set spindle coiling draw ratio in 70 to 500 scope,

B) monofilament comes out from spinning head, and the back is direct passes 30mm to the long quenching time-delay district of 200mm with its conveying,

C) monofilament is quenched into below the solidification temperature,

D) on the distance of 2500mm, compiling monofilament from spinning head lower surface 500mm,

E) set before the traction draw-off godet and between yarn tension be 0.05cN/dtex between the 0.20cN/dtex,

F) with 0.025cN/dtex to the tension winding yarn between the 0.15cN/dtex.

20. the process of claim 1 wherein that winding speed is set between 2200m/min and the 6000m/min.

21. the process of claim 1 wherein that the operating characteristic viscosity number is at PBT and/or the PTMT of 0.7dl/g in the scope of 0.95dl/g.

22. the partially oriented polyester multifilament yarn that the method by claim 1 obtains is characterized in that under as German standard DIN 53802 defined standard conditions after 4 week of storage

A) extension at break is between 75% to 145%,

B) boil-off shrinkage is in 0 to 10% scope,

C) nominal Uster is lower than 1.1%,

D) breaking load variation coefficient≤4.5% and

E) extension at break variation coefficient≤4.5%.

23. be used to produce the method for fluffy yarn, wherein be at least the polyfilament yarn of handling claim 22 in the draw texturing machine of 500m/min in speed.

24. the polyester SET monofilament that can obtain by the method for claim 31, it is characterized in that its fracture strength greater than 20cN/tex and elongation at break greater than 32%.

25. the polyester HE monofilament that can obtain by the method for claim 23, it is characterized in that its fracture strength greater than 20cN/tex and elongation at break greater than 30%.