DK143073B - PROCEDURE FOR THE PREPARATION OF A POLYESTER YARN - Google Patents

Description

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This invention relates to a process for producing a textured polyester yarn in which a polyester is melt-spun to form an unstretched filament bundle as a starting material, upon which this material is subjected to a stretch-peel-wrinkle texturing treatment.

Polyester filament yarns have so far been made by melt spinning at relatively low speeds of approx. 1000 meters per minute or less, followed by stretching of the filaments in a separate step. Up-10 winding means that can operate at up to 4000 meters per has been available and has been used commercially to recover fully stretched yarns made by said two-step method comprising melt spinning to form cooled solid filaments 15 at a relatively low rate, followed by stretching, e.g. 3.5 times, and then recovering the fully stretched filaments using said high-speed inventions.

In the disclosure of U.S. Patent No. 2,604,689 20, it has been proposed to produce, in the spun condition, tough polyester filaments by a one-step method comprising high-speed spinning instead of the commercially used practice, first spinning at low speeds and then making stretch to improve the mechanical properties of the filaments. However, high speed spinning of polyester filaments has never been commercially accomplished.

Most polyester multifilament yarns are textured to improve yarn volume and grip. The preferred commercial method of texturing comprises falsification and heat curing of the thermoplastic yarn. So far, the fake cleaning process has only been commercially done with fully stretched food yarns.

It has long been suggested, e.g. in British Patent Specification No. 777,625 and in United States Patent No. 3,279,164 that the false swirl texturing process could be combined with the stretching process. Conventional counterfeit texture texturing apparatus (designed for use with fully stretched yarns) can be readily modified to include stretching, either by reducing the speed of the feed roller or by replacing the roller with voltage generating means. . No success has been achieved in this way with non-stretched nylon yarns, but so far the process has never yielded good results with unstretched polyester yarn. It is conventional to use heater temperatures in excess of 200 ° C in the false-sheave texturing of fully stretched polyester food yarns because at the higher heater temperature a better ripple is obtained.

However, it has been found that when non-stretched polyester feed yarn is textured false using such high heater temperatures (which are conventional for fully stretched feed yarns), the yarn 15 overheats and breaks or melts. This makes it difficult or impossible to thread the machine, cf. Dutch Patent Application No. 69.02331, which discloses a typical known method for stretching false-shaving texturing.

The present invention relates to a method in which these and other deficiencies of the above-described technique are remedied or minimized as possible, in the manufacture of a textured polyester yarn by which a polyester is melt spun to form an unstretched filament bundle as a starting material. , wherein this material is subjected to a stretch-falseness texturing treatment, and this method is characterized in that oriented filaments are prepared by withdrawing the polyester from the spinning nozzle at a rate of at least 2750 m / minute, wherein the bundle of filaments 30 contains a surface modifying agent to reduce the frictional properties of the starting material so that the coefficient of friction between the filaments does not exceed 0.42 as measured below, and that the starting material of the stretch-false-spun texturing treatment is stretched to a ratio greater than 1, 3: 1 to a maximum of 2: 1, the twist being fixed with a heating means at a temperature above 200 ° C.

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The method according to the invention is further illustrated with reference to the drawing, which shows a diagram of the present-day stretching false-texturing operation.

5 At the stretch, a polyester yarn 1 is continuously fed from a yarn roll by means of feed rollers 3 and 3. The polyester yarn is passed through a texturing heater 4 and a false twisting member 5. It is pulled off by rollers 6 and 6 'and retrieved on a yarn roll 7. The false twisting member 10 rotates at a high speed, giving "S" twists on one side of the member and " Z ”twists on the other hand. The coils return to the feed rollers 3 and 3 'so that the yarn is in a twisted state as it is passed through the heater 4. The heating plasticizes the polyester-15 yarn and causes crystallization. After cooling, the twisted configuration of the crystallized molecular arrangement is fixed. The yarn is cut off as it is guided from the false prong to the rollers 6 and 6 '. Rollers 6 and 61 move at a higher peripheral speed than feed rollers 20 3 and 3 'to obtain a suitable stretching ratio. This method is referred to herein as a "simultaneous" stretching false twist texturing method because the yarn is stretched in the twisting zone. Commercially available texturing machines can be modified to operate by the method of the invention by decreasing the speed of rollers 3 and 3 'and / or by increasing the speed of rollers 6, 6' to obtain the necessary stretching ratio.

The yarn is then fed to the yarn roll 7, which is usually driven at a somewhat lower peripheral speed than the rollers 6 and 6 'to avoid excessive tension in the yarn on the yarn roll. Other heating means (not shown in the drawing) may be used between the stretch rollers and the yarn roll to stabilize the textured yarn and reduce its twisting viability such as e.g. disclosed in United States Patent Nos. 3,131,528 and 3,316,705.

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Optional rollers 8 and 8 'are indicated by dashed lines between the feed rollers 3, 3' and the texture heater 4. These rollers can be used when working with separate stretching and twisting zones. For example, when if lower stresses are desired in the false-shaving texturing operation, the peripheral speed of the rollers 8, 8 'may be higher than the speed of the rollers 3,3'. Such a process is herein referred to as the "tandem" or "sequence" stretching false truncation texturing process. The relative velocities of the rollers 3, 3 ', 10 rollers 8, 8' and rollers 6,6 'can be adjusted to obtain. a tandem process with some simultaneous stretching. If desired, a heater can be inserted into the stretching zone between rollers 3, 31 and rollers 8, 8 ', but usually a stretch heater is not required in a tandem process.

In the method of the invention, oriented polyester filaments are made by melt spinning at very high spinning rates. Conventional commercial conditions and apparatus for melt spinning of polymers are applicable to the point where the molten polyester 20 leaves the spinning nozzle in the form of filaments. The filaments are then immediately quenched with a cooling gas. As the filaments cool, they are pulled from the spinning nozzle at a rate much higher than usual.

This causes the filaments to become very diluted before reaching the peel members. The cooled filaments can then be directed to a winding means, e.g. by means of high speed peel-off rollers at essentially the same speed with which the filaments are wound on the yarn roll. The rate at which the filaments pass through the peel rollers is herein referred to as the "peel" speed.

The process does not require a conventional stretching step. The cooling requirements of the filaments depend, among other things, on the configuration of the particular cooling zone and apparatus, the spin rate, the denier value and the filament number, but can be readily determined by tests as is well known in the art.

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The preferred polyesters for use in the process of the invention consist of at least 90 mole percent polyethylene terephthalate. The particularly preferred are mainly polyethylene terephthalate. As with a conventional polyester yarn manufacture, the polyester filaments may contain minor amounts of conventional matting agents, particulate matter, antistatic agents, optical brighteners, antioxidants, and copolyester components.

The process is preferably carried out at a 2-0 draw rate of 2750 to 3200 meters per second. minute.

This speed, combined with good cooling conditions, has been found to provide filaments with optimum properties for the subsequent stretching-falsification texturing by the method of the invention. A much faster * * -5 higher withdrawal speed can be used, but a withdrawal speed of less than 4100 meters per second. Minutes are usually preferred to avoid too many fractures of the molten filaments as they emerge from the spinning nozzle. Other high-speed spinning processes are described, e.g. in U.S. Patent Nos. 20,604,689 and 3,053,611, but these patents do not contain, nor suggest, conditions for making a food yarn suitable by a stretching and texturing method.

By appropriate selection of the withdrawal rate 25 and the cooling conditions of the extruded melt spun polyester, filaments with the desired birefringence, fracture elongation and crystallinity are obtained. As with conventional melt spinning methods, the filaments are combined in freshly spun to form a yarn which, in the method of the present invention, is the feed yarn for the subsequent stretching false spun texturing operation. The desired rubbing properties between the filaments in the feed yarn can be obtained by incorporating in advance a suitable surface modifier in the polyester melt 25 or by using e.g. a lubricant on the surface of the filaments or using both methods.

As will appear from the following, the treatment with said agent must be carefully selected to obtain the desired rubbing properties.

The polyester yarn made at the above-described steps is then ready for stretch-false-trimming texture.

For convenience, the yarn can be wound onto a yarn roll ^ before the texturing operation. Further for convenience, the gamut may be intertwined prior to texturing by passing through a nozzle which e.g. placed immediately after the pull-off rollers. An interlacing number of 10 to 150 cm, explained with a stick, is explained below.

10 Above the value of 150 cm, the filaments in the yarn may under certain conditions be entangled and thereby cause difficulties in subsequent machining. Below a number of sticks of 10, the yarn becomes so closely intertwined that the subsequent stretching of the yarn is, in some conditions, prevented by the stretching false-shaving texturing operation.

The polyester food yarns may be subjected to simultaneous or tandem (i.e., sequential) stretching false-trimming texturing operations. The yarns are stretched by the stretch-fold twist-texturing operation to a ratio of 20 from above 1.3: 1 to at most 2: 1, the induced twisting of the yarn being fixed with a heater at a temperature above 200 ° C. . Temperatures above 200 ° C give the textured yarn the desired evolution of ripple as defined below, while the ripple below 200 ° C is usually insufficient.

In the stretch texturing operation, the minimum twist to be given to the yarn increases with decreasing yarn denier. Usually the stretch texturing machine is set to produce a twist in the yarn at turns 30 per minute. 2.5 cm, numerically equal to or greater than 7 34 x 10 ^ - - 10, where D is the denier value of the yarn before

Vd "texturing. In the process of the invention it is possible to produce textured yarns with a ripple evolution at a load of 2.5 mg per denier which is numerically equal to or greater than 22-0.05 (D '). The ripple development (CD2 5) for a 70 denier yarn, for example, would be greater than 0 7 143073 18.5 and for a 400 denier yarn greater than 2. Food yarns with a denier value of 100 -300 is preferred.

It is surprising by the present invention that it is now possible to stretch non-stretch textured non-stretched polyester food yarns in freshly spun condition on commercial machines with only minor modifications.

It is also surprising that the textured yarns thus produced have properties such as ripple development, voluminosity and twisting properties that are superior to conventional polyester yarns made with similar twists and hot plate temperatures. Other advantages of the present process are high work rate and productivity of the texturing operation and good uniformity of the coloring 15 of the textured yarns.

In the process of the invention, it is particularly desirable that a non-stretched polyester yarn having a double breaking of at least 0.025 (i.e., with molecular orientation), a fracture elongation of between 70% and 180% and a crystallinity of less than 30% are subjected to stretch-falsification. texturing. Indeed, it has been found that such a food yarn is particularly suitable for the stretch-falseness texturing. Such a food yarn is quite different from known conventional polyester yarns. Conventional freshly spun polyester yarns that are not stretched, for example, although low crystallinity, are completely unoriginal. Other conventional polyester yarns, although oriented, have a higher crystallinity. A further key feature of the feed yarn, which distinguishes it from other yarns, is its low coefficient of friction between the filaments, which will be discussed below.

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It was surprising to find that the polyester food yarns preferred by the method of the invention not only provide increased productivity and better ripple development in the stretch-fold cleaning texturing operation, but that the food yarns themselves have unexpected advantages in storage stability. Thus, the yarns can be stored prior to texturing for more than 600 days without any noticeable deterioration in the practice of stretching texturing. Southwestern restructuring.

Although the process proceeds satisfactorily when the feed yarn has a coefficient of friction between the filaments of less than 0.42, the resulting textured yarns often have several filaments that are broken (ie, measured by a "broken fiber number") - These textured yarns are usable for use in the manufacture of many double knit goods. However, when knitting knitwear, the requirement regarding the number of broken filaments is much stricter. It has been found that when the coefficient of friction between the filaments in the feed yarn is kept at a value no higher than 0.37.25 satisfactory textured yarns can be produced for knit knitting. Even more preferred are yarns with a coefficient of friction between the filaments of not more than 0.34. These provide textured yarns with very few broken filaments. A coefficient of friction between the filaments 30 of more than 0.2 is also preferred to avoid slippage of sections of twisted yarn after the crease spindle during the stretching crease texturing operation and a consequent non-uniformity in the textured product.

Thus, in the method of the invention, it is appropriate to incorporate in the filament bundle a surface modifier which gives the non-stretched starting yarn a coefficient of friction between the filaments of not more than 0.37, preferably between 0.2 and 0.34.

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As indicated by the description of the process of the invention, the low coefficient of friction between the filaments is obtained by incorporating a surface modifier into the polyester melt prior to spinning or using a lubricant in the feed yarn. Although many such agents have been investigated, only a small number have been found suitable for production. of a coefficient of friction between the filaments of not more than 0.37. When agents such as polyoxyethylene glycol having a molecular weight of 20,000 or pyrophosphate-coated kaolinite are incorporated into the polymer prior to spinning, it is possible to satisfactorily use typical lubricants usually proposed for conventional texturing of yarn to produce it by the method of preferred food yarns.

A low frictional value for the feed yarn filaments on the spindle surface is advantageous to avoid excessive tension in the filaments.

In addition to the friction properties discussed above, there are a number of other important properties of the preferred polyester food yarns. The preferred food yarns have a structural integrity parameter, as defined below, of no more than 1.0. It is also preferred that the structural integrity parameter is not less than 0.3.

A break elongation of at most 180% for the polyester filaments 25 in the feed yarns is suitable for use in the method of the invention, and it is preferred that the elongation at break is not less than 70%. With a structural integrity parameter greater than 1.0 or a fracture elongation greater than 180%, the food yarns are very difficult, if not impossible, to step on the stretch-false-trimming texturing machine.

A feed yarn with a structural integrity parameter of less than 0.3 or a fracture elongation of less than 70% requires such high spin rates that filament rupture occurs in the molten filaments when extruded. Accordingly, such filaments 35 cannot be produced with the efficiency obtained when operating within the preferred limits. The preferred ranges of 0.4 to 0.9 for the structural integrity parameter and 109-176% for the fracture elongation provide food yarns, which work most effectively in the subsequent stretch-falseness texturing operation. For the most effective operation, it is also preferred to use food yarns with a shrinkage after boiling, as described below, at least 40%. It is also preferred that the shrinkage after boiling is not more than 60%. It is further preferred that the yarns have an interlacing number determined by a stick of 10 to 150 cm. In order to achieve the desired degree of interlacing in the final textured product, the interlacing rate of the food yarns must be higher than the interlacing rate of a conventional fully stretched yarn, probably because the distance between the interlacing knots is extended during the stretching and twisting of the yarns in comparison to a purely twisting yarn. of the 15 conventional yarns during texturing.

The method according to the invention provides stretch-false-twist textured polyester yarns which are novel. The filaments in these stretch-textured yarns have two unusual properties, namely the measured values of their denier-20 variations and their birefringence difference, both defined below.

With regard to denier variation, it has been found that filaments of yarns textured according to the above-described false-cut texturing method and according to the prior art denier variations exhibit along their length. The variations occur at a frequency of approx. 1/3 of the degree of twist used in texture. Therefore, if the degree of rotation is 24 rpm. cm, the denier value varies approx. for each 0.13 cm. Textured polyester yarn, made by first stretching conventional polyester filaments and then falsifying the textured ones, has a variation around the mean denier value of less than + 6%. Textured polyester yarn made by feeding with conventionally spun non-stretched polyester yarn to a texturing machine and then stretching at least 2 times during texturing has a variation around the mean nerve value of more than + 12%. By comparison, the filaments of the textured yarns made by the method of the invention exhibit a denier variation of less than + 12% and more than + 6%. Denier variation is influenced by the degree of twist, temperature and applied voltage in the texture zone of the texturing machine.

With regard to the birefringence difference, it has been found that the birefringence near the surface of the filament is significantly higher than near the center when the polyester filaments are extruded at the high speeds required by the method of the invention. This difference is also noticeable after the fibers have been stretched-fold-cut textured, and is at least 0.008. The filaments in false-sheave textured polyester yarns made by known methods have double refraction differences well below this value of 0.008.

In order that the textured yarns made by the method according to the invention can be used in many different ways in the textile industry, it is preferred that they have a tensile strength of at least 2 grams per minute. denier. It is also preferred that these yarns have a nominal break elongation of 20-35%.

20 Several parameters have been used to characterize the food yarns and textured products. These parameters are defined together with the methods for their measurement in the following sections. Further methods used in the examples to measure other properties of the yarns are also given.

The coefficient of friction between the filaments is a measure of the ease with which the filaments slide side by side.

Ca. 690 meters of yarn is wound back and forth around a cylinder with a winding angle of + 15 ° and a winding voltage of approx. 10 grams. The cylinder has a diameter of 5.1 cm and a length 30 of 7.6 cm. 30.5 cm of the same yarn is placed over the cylinder so that it rests on top of the wound yarn and is parallel to its turns. A weight in grams equal to 0.04 times the denier value of the overlay yarn is connected to one end of the overlay yarn and a deformation measuring apparatus 35 is connected to the other end. The cylinder is then rotated 180 ° at a circumferential speed of 0.0016 cm. second, so that the deformation meter is under voltage.

The voltage is read continuously. The coefficient of friction 12 between the filaments, f, is then calculated by the following equation derived from the well-known equation for the friction of a belt running over a cylinder.

5 f = 1 ln IT2 [T1] 7Γ where T2 is the mean of at least 25 read peak voltage values, the voltage is obtained with the weight connected to the yarn and ln is the mathematical symbol of the natural logarithm. Results from yarn samples that have a permanent extension during the test are not used. All results are measured at 70 ° C.

Fracture elongation and tensile strength are measured in accordance with the provisions of ASTM under D-2256-69. The tests are done with just 15 multifilament yarns conditioned at a relative humidity of 65% and 21.1 ° C for 24 hours prior to the experiment. An Instron voltage test machine is used. The test specimen is 12.7 cm long.

No twisting is added. The cross head speed is 25.4 cm per and the degree of attenuation is 200% per minute. minute. Diagram 20 speed is 12.7 cm per minute. The tensile strength is the maximum load in grams before yarns break, divided by the denier value of the yarn.

Double breaking and crystallinity are measured by a conventional technique, such as in U.S. Patent No. 2,931,068, 25 column 4, line 17 - column 5, line 5. Since the crystallinity of the yarns is usually much lower than 30%, conventional density measurements are usually sufficient to show this.

Viscosity fraction n a measure of the molecular weight of the polymer is the ratio of the viscosity of a solution of 0.8 grams of polymer dissolved at room temperature in 10 ml of hexa-fluoroisopropanol containing 80 ppm E 2 SO 2 to the viscosity of the H2 SO4-containing hexafluoro isopropanol. self.

Both viscosities are measured at 25 ° C in a capillary viscometer.

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The shrinkage after boiling is achieved by suspending a weight in a yarn length to obtain 0.1 mg / denier load of the yarn and measuring its length L. The weight is then removed and the yarn immersed in boiling water for 30 minutes. The yarn 5 is then removed from the water and loaded again with the same weight and its new length measured L ^. The shrinkage after boiling is calculated as a percentage according to the formula:

Shrinkage after boiling = L ~ Lf x 100

10 L

The structural integrity parameter (£) can be used in conjunction with poly (ethylene terephthalate) homopolymer and measured as follows. A weight is hung in a length yarn to obtain a load of 0.2 grams per second. denier of the yarn.

The length of the loaded yarn is measured. The yarn is then immersed in water at 100 ° C for 2 minutes and carefully removed from the water and cooled. Then its length is measured again.

All these steps are carried out with the yarn carrying the load 20 caused by the weight. The structural integrity parameter is then calculated by the equation.

In contrast to food yarns used in the process of the invention having values of 0.3 to 1.0, conventional polyethylene terephthalate blanks stretched after the spinning have negative o values. The feed yarns 30 can be prepared by a known method.

The denier variation in the filaments of the textured yarn can be measured using a Viviani measuring apparatus, as proposed in Rowland Hill, "Fibers from Synthetic Polymers". Elsevier Publishing Co., London (1953), page 383. This method of determination is based on a measurement of changes in the conductivity of an electrolyte in a fine capillary tube while a filament is passed through the capillary tube.

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The double refraction difference, 6, is defined here as the difference between the average birefringence near the surface of the fiber and the highest birefringence in the fiber near its center. This definition is best understood from the way in which it is measured.

A dual current interference microscope, such as negotiated by E. Leitz, Westzlar, A.G., is used. The fiber to be examined is immersed in an inert liquid with a refractive index nT different from the refractive index of the fiber with an X0 amount giving a maximum displacement of the 0.2 to 0.5 wavelength interference lines. The value of nL is determined with an Abbe refractometer calibrated for sodium D light and not corrected for green mercury light used in the interferometer. The fiber is placed in the liquid such that only one X5 of the double currents passes through the fiber. The fiber is oriented with its axis perpendicular to the non-offset lines and the optical axis of the microscope. The pattern of the interference lines is plotted on a T-410 polaroid film with a magnification of 1000 times. The line offsets are associated with the refractive indices and fiber thickness according to the following equation: d _ (n - nL).

z in which 25 n is the refractive index of the fiber is the wavelength of the light used (0.546 fi), d is the line offset, D is the distance between adjacent lines, and t is the length of the light path (i.e., the fiber thickness, at the point where d is painted.

For each line offset, d, as measured on the film, a single n and t apply. To determine the values of the two unknowns, measurements are taken in two fluids, preferably one having a higher and one having a lower refractive index than the fiber of the above specified criteria. Thus, for each point along the width of the fiber, two sets of data are obtained from which n and t are then calculated.

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The birefringence ,. - (Λ η), by definition is the difference in the refractive index of polarized light perpendicular to the fiber axis (n_L) and to light polarized parallel to the fiber axis (n), i.e. (Δη) = (η - η I). Dobbeltbrydningsforskel-

II II

leno is then calculated as the difference between the birefringence near the fiber surface, (^ n) g, (i.e., at a point offset transversely from the fiber axis by at least 0.95 r, where r is the fiber radius) and the birefringence at the extremity of the fiber core (4n) c (i.e., at a point that can be located between the fiber center and 0.65 r). The double refraction at the extremity is a minimum for the high-surface double-break fibers and is a maximum for low-surface fibers - double-break.

15 X all of the above calculations are all linear dimensions in the same units and converted if necessary either to the enlarged units in the photograph or to the absolute units on the fiber.

The pin number determined by pin, as defined herein, is the length of a yarn in cm that passes through sample 18 of U.S. Patent No. 3,290,932 before deflecting the sample approximately. 1 mm. An 8 gram force is required to deflect the sample.

The number of broken filaments is determined by an optical technique in which the yarn passes along and perpendicular to an intense luminous flux. Broken filaments entering the light stream reflect a light pulse that is captured, amplified and reproduced at an appropriate counter. The figure is stated here as broken filaments per. 183 meters of textured yarn.

The process of the invention is further illustrated by the following examples, in which all percentages and parts are percentages by weight and parts by weight, unless otherwise stated. In each of the examples, the polyester yarns are textured in a commercial Leesona 570 false swatch texturing machine, as described in U.S. Pat.

3292354. The machine is modified so that the yarn is stretched during texturing. The yarn is fed from a yarn roll by means of feed rollers, passes up along a heating plate to a crease spindle and is pulled away by upper rollers driven at a higher speed so that the feed rollers extend the gamut. The increase in speed is achieved by means of different gears. The hot plate in the twisting zone usually has a temperature of 216 ° C. The spindle speed is 270,000 rpm. minute to produce approx. 24 rpm cm in the yarn when the yarn moves at a speed of approx. 114 m per minute. The textured yarn is then stabilized by passing from the upper rollers with an overfeed of 14.5% to a top heater operating at a temperature of 213 ° C. The yarn is then wound up on a yarn mile with an overfeed of -4% (ie under light tension). Stretching conditions and stresses in the up and down direction of the spindle are measured.

In each of the following examples, unless otherwise mentioned, the polyester yarns made for feeding the stretch false-false texturing apparatus described above have a fracture elongation of less than 180%, a crystallinity well below 30% and a birefringence of at least 0.025. To facilitate comparison, each multifilament yarn has 34 filaments. In Examples 1-4, the filaments are melt-spun at 302 ° C from a spinning nozzle with 34 round openings, each having a diameter of 0.23 mm and a length of 0.31mm. The freshly spun filaments are cooled abruptly in a vigorous flow of air at a temperature of 21 ° C, passed to a pair of high speed stretch rollers located approx. 6 meters below the spinning nozzle, make five turns on these rollers and then pass through a braid nozzle which is supplied with air at room temperature at a pressure of 2 1.4 kg / m to produce a braided yarn having an interlacing number determined by pin of 102 cm. The yarn is then wound 20 with a usual yarn winding tension. The winding rates (virtually identical to the spin removal rates) of these examples are given in Table 1, together with other important data for the polymers used, the food yarn produced, the texturing conditions and the final textured food yarn.

Textured yarns made according to the following examples usually have a tensile strength of well over 2 grams per second. denier, a birefringence difference of at least 0.008, and a variation in the mean filament denier value of less than + 12%, but somewhat 0 + 17% higher than + 6%.

Example 1

Three polyester food yarns denoted by I-a, I-b and I-c prepared as described above from polyethylene terephthalate containing 0.27% by weight TiO 2 matting agent. Each of the yarns is melt spun from spinning nozzles at approximately the same speed, but is wound up and drawn at different rates, as shown in Table I, to form feed yarns with fracture extensions of 133, 165 and 10, 198%, respectively. It should be noted that the feed yarn I.-c is melt spun at less than 2750 m / minute and therefore serves for comparison.

The yarns lubricant is treated by passing the filaments in sliding contact over a cylindrical lubricant roller disposed in the upward direction from the peel rollers. This lubricant roller has a diameter of 11 cm and a length of 10 cm and consists of Alsimag ^ 614 (a product of American Lava Corp.) · The lubricant treatment is also carried out immediately downwards from the peel rollers with a roller having a diameter of 10 cm and a length of 2.5 cm 20 and consists of AXF-T9V 500-grit glassy tape (a product of Norton Corp.). The applied lubricants are like those described in U.S. Patents 3,563,892 and 3,338,830 and are made as follows:

A mixture is prepared in a 25-vapor stainless steel container from 65.0 parts of coconut oil, 20 parts of the sodium salt of glyceryl trioleate as an aqueous 75% solids (15 parts dry weight), 10 parts of a material made by condensing a molecular part nonylphenol with 5-6 molecular parts ethylene oxide, 10 parts of a mixture 30 of mono- and diglycerides of oleic acid and 1 part of oleic acid. The mixture is stirred while the temperature is raised to 50 ° C and 1 part of triethanolamine is added. Then, polyoxyalkylene glycol, which is 5% by weight of the non-aqueous ingredients in the above mixture, is dissolved in water heated to 50 ° C. This solution is then added to the above mixture. The polyoxyalkylene glycol contains oxyethylene and oxy-1,2-propylene groups in a weight ratio of 3: 1 and has a viscosity of 20,000 centipoise at 37.8 ° C. The resulting lubricant is applied as a 5-10% aqueous emulsion as 0 18 1473. After evaporation of the water, the yarns on their surface have the weight percent of lubricant listed in Table I. This treatment gives each of the yarns a coefficient of friction between the filaments of 0.26.

5 The yarns are stretched-false-cut textured under the conditions described above and as further indicated in Table I. The yarns Ι-a and I-b are stretched without difficulty and satisfactory products are obtained in all essential respects. However, the feed yarn I-c (comparison) with its high break-10 elongation of 198% and its high structural integrity parameter of 1.06 cannot be treaded on the machine in a normal way because the yarn melts. This yarn must therefore be removed from the heater during threading and the first operation. This is a difficult procedure that gives waste product and 15 unwanted unused time.

Example 2

Three yarns denoted by Il-a, ΙΙ-b and II-c are prepared and stretch-textured as in Example 1, except that another lubricant is applied which gives the yarns a coefficient of friction between the filaments of 0.42 as compared to 0 , 26 for the corresponding yarns of Example 1.

The lubricant used in this example is a two-layer combination that has been used exclusively in conjunction with fully stretched polyester food yarns in conventional texturing processes. The agent applied upwardly from the peel rollers is disclosed in U.S. Patent No. 3,428,560 and is a 10% aqueous mixture containing 49 parts of 30 isocetyl stearate, 24.5 parts of sodium di- (2-ethylhexyl) -sulfo-succinate, 24.5 parts of a condensation product of 1 mole of stearyl alcohol and 3 moles of ethylene oxide, 1 part of triethanolamine and 1 part of oleic acid. 0.1% after drying, based on the weight of the yarn.

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Just prior to winding, the yarn is treated with another conventional lubricant which has been completely satisfactory when applied in this way to fully stretched food yarns by conventional counterfeit texturing processes. It is an aqueous mixture Containing 20.5 parts of sulfated peanut oil, 1.8 parts of diethylene glycol, 1.8 parts of potassium hydroxide, 62.6 parts of an ester of 1-butanol and a 45-55 mixture of stearic and palmitic acid, 8 , 2 parts oleic acid, 3.4 parts triethanolamine and 1.7 parts orthophenyl-phenol. This second lubricant is applied in an amount of 0.2-0.3% of agent to the yarn after drying.

As shown in Table I, the textured yarns of Example 2 with their much higher friction between the filaments have a much higher number of broken filaments than the corresponding yarns of Example 1. Although the textured yarns with such a high number of broken filaments are suitable for somewhat knitted material, yarns with much lower numbers are desired in order to be used in the manufacture of many more materials. As also with yarn I-c, the feed yarn 20 II-c, which represents a scissor comparison experiment, with its high fracture elongation, cannot be processed on the stretch texturing machine without the yarn being removed from the heater during threading and initial processing.

Example 3

This example demonstrates the beneficial effects of having polyoxylethylene glycol in the polyester in the food yarns.

A yarn is made from polyethylene terephthalate 30 containing 0.27% TiC> 2 and 5.5% polyoxyethylene glycol ("PEO") having a molecular weight of 20,000. (Polyester yarns containing PEO are described in British Pat.

956,833). With the exception of the PEO addition, essentially the same food yarn preparation, lubricant processing and stretch-falsification texturing are used as in Example ΙΙ-b. However, as a result of PEO in the polymer, the food yarns of this example, unlike the yarns of Example II-b, have a much lower coefficient of friction between the filaments (i.e., 0.22 to 0.42) and therefore have a much lower number broken filaments in the textured yarn (i.e. 7 vs. 185).

5

Example 4

This example demonstrates the beneficial effect of having pyrophosphate-coated kaolinite in the food yarns.

In this example, yarns are prepared from polyethylene terephthalate containing 0.27% TiC 2 and 1.72% of the pyrophosphate coated kaolinite disclosed in Example 1 of U.S. Patent 3,376,249. In all other ways, the yarn preparation, the lubricant treatment and the stretch-false wrap texture are the same as in Example IIa. However, as shown in Table I, the yarns of this example are textured with kaolinite in the polymer much better than the yarns of Example IIa (i.e., 6 vs. 147 broken filaments) as a result of the much improved coefficient of friction between the filaments (i.e. 0.27 versus 0.42).

Example 5

A yarn is prepared from polyethylene terephthalate / 5-25 (sodium sulfone) isophthalate (molar ratio 98/2) containing approx. 0.45% by weight of TiC 2 - With the exception of the copolymer, lubricant and texture-stretching ratio, the yarn is prepared mainly as in Example I-a.

The lubricant applied is a mixture of 35.5 parts by weight of 30 coconut oil, 18 parts of the tetraoleate laurate pentester of the condensate of 1 mole of sorbitol with approx. 30 moles of ethylene oxide (described in U.S. Patent No. 3,421,935), 7 parts of hexaglycerol tristearate, 2.5 parts of aluminum hydroxystearate, 5.5 parts of a reaction product of 2 parts of a secondary alcohol of 10-12 carbon atoms, and 3 parts of ethylene oxide , and 31 parts of polyoxyalkylene glycol. The polyoxyalkylene glycol contains oxyethylene and oxy-1,2-propylene groups in the 3: 1 weight ratio and has a viscosity of 20,000 centipoise at 37.8 ° C.

0 143073 21

The lubricant is applied to the yarn in an amount of 0.24%, based on the weight of the yarn. The yarn having a coefficient of friction between the filaments of 0.33 is processed in all respects satisfactorily in the stretch texturing machine and provides textured products with the desired properties, e.g. relative to I-c that cannot be stepped.

Three other lubricants which give the yarns coefficients of friction between the filaments of 0.27 to 0.30 when applied in an amount of approx. 0.3 to 0.4% and permits a good practice of the low-stretch stretch fabrication texture with low number of broken filaments are as follows: 1. A mixture of 11 parts of the polyoxyethylene glycol used in this example, 72.5 parts of diundecyl phthalate, 11 , 7 parts of sulfated peanut glycerides 15.5 parts of a condensate 15 of 1 mole of nonylphenyl with 5 to 6 moles of ethylene oxide and approx.

0.3 parts potassium hydroxide.

2. A mixture of 50 parts of coconut oil, 30 parts of the sorbitol condensate of US Patent No. 3,421,935 used in this example and 20 parts of a soft hydrocarbon wax having a melting point of approx. 34 ° C and is composed of a mixture of high molecular weight and naphthenic wax naphthen oils.

3. A mixture of 50 parts of ditridecyl adipate, 35 parts of the sorbitol condensate described in U.S. Pat.

3,421,935, 5 parts of nonylphenol, ethylene oxide condensate (molar ratio 1: 5 to 1: 6) and 10 parts of the polyoxyalkylene glycol used in this example.

Example 6 Polyethylene terephthalate containing 0.3% TiO 2 is melt spun at 289 ° C from a spinning nozzle with 34 round openings, each having a diameter of 0.51 mm and a length of 5.1 mm.

The freshly spun filaments are cooled abruptly as in Examples 1-5 and extracted at a rate as given in Table I.

A lubricant is applied to the yarn as described in Example 1 using a 10% aqueous mixture. The lubricant is of the usual type described in U.S. Pat.

3,594,200 and contains 36.3 parts of the sodium salt of one

ISLAND

Sulfated peanut oil, 27.5 parts refined coconut oil, 1.9 parts potassium hydroxide, 24.5 parts aromatized phosphate ester and 9.8 parts soft hydrocarbon wax. Properties of the prepared food yarn and the satisfactory stretch wrinkle-textured product made from this yarn are given in Table I.

23 143073

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