US 3859122 A
Improved feed yarn for draw-texturing has a finish composed of about 55 parts by weight of an ester oil lubricant, about 45 parts of a nonionic surface-active emulsifier, and about 0.6 to 2 parts of poly(oxyethylene-oxy-1,2-propylene) glycol having a viscosity of about 9,000 SUS. A preferred ester oil is di(tridecyl) adipate. A preferred emulsifier is a tetraoleate-laurate of a condensate of sorbitol with ethylene oxide, plus a small amount of a condensate of nonylphenol with ethylene oxide. Twist slippage and broken filaments are reduced to provide uniform textured yarn, and objectionable deposits on equipment are avoided.
Description (OCR text may contain errors)
United States Patent 1191 Burks, Jr, et a1.
1 1 FISH COMPOSITION FOR DRAW-TEXTURING YARN I751 Inventors: Philip I. Burks,,1r., Grecnville,
N.(.; Quinton Cooke, .1r., Hcndersonvillc, 'l'enn.
 Assignee: E. l. du Pont de Nemours and Company, Wilmington, Del.
22 Filed: Feb. 1, 1973 21 Appl.No.:328,851
 US. Cl. ll7/l38.8 F, 117/l38.8 N, 1l7/138.8 E, 117/139.5 CQ,
 Int. Cl. D06m 13/18, D06m 13/20  Field of Search 28/726,,75 WT; 57/140, 57/149,153;1l7/l38.8 F, 139.5 B, 139.5
CQ, 139.5 F; 252/89  References Cited UNITED STATES PATENTS 3,042,544 7/1962 Marzocchi et a1. 117/72 3,306,850 2/1967 Olsen 1. 252/87 3,338,830 8/1967 Stokes et al. 252/89 3,421,935 1/1969 Finch 117/138.8 3,464,922 9/1969 Bernholz et a1... 252/86 3,641,073 2/1972 Buckley 260/4106 14 1 Jan. 7, 1975 3,687,721 8/1972 Dardoufas 117/138.8F 3,704,225 11/1972 Shay ..252/8.9
OTHER PUBLICATIONS The O. G. Defensive Publication Finch Def. Pub. of Ser. No. 791,501, filed Jan. 15, 1969, published in 878, 0.0. 1147, on Sept. 29, 1970, Def. Pub. NO. T 878,012. Ucon-Fluid and Lubricants; Union Carbide Chem., NY.
Primary Examiner-P. E. Willis, Jr.
57 ABSTRACT 1 Claim, N0 Drawings FISH COMPOSITION FORDRAW-TEXTURING YARN BACKGROUND OF THE INVENTION running it over a heater, at temperatures of up to 240C., to a false-twist spindle having a rotational speed of up to 500,000 rpm. Finishes are applied to the surfaces of the yarn filaments to lubricate them, protect them from abrasion and heat damage, and minimize accumulation of electrostatic charges. In the performance of these functions, the finish should not smoke, fume or form solid deposits on the equipment. From an ecological point of view, the finish should be biodegradable and not contribute to environment pollution. Finishes have been devised that satisfy the requirements for producing high quality textured yarn from previously drawn yarn, such as finishes disclosed in Stokes et al., US. Pat. No. 3,338,830, dated Aug. 29, 1967. v
Many attempts have been made to combine the operations of drawing and false-twist texturing in a single drawtexturing process which starts with an undrawn or incompletely drawn feed yarn. Textured yarns produced by such processes have repeatedly exhibited non-'uniformities and broken filaments, particularly when polyesteryams are draw-textured on modern machines at relatively high heater temperatures and rotational speeds of twisting devices. It has now been found that previous finishes are inadequate for this purpose. For example, the surface friction of the filaments must be lowenough toavoid broken filaments, but not so low that there is twist slippage during the false-twisting operation. If twisted yarn slips past the false-twisting spindle, it will cause defects in the textured yarn. Problems with previous finishes are overcome by the present invention.
SUMMARY OF THE INVENTION The improved synthetic textile yarn of the present invention has from 0.1 to 1.5 percent (preferably 0.2 to 1 percent) by weight based on the weight of the yarn, of a finish composed of the following:
a. 50 to 60 parts by weight of an ester oil lubricant of the general formula R(ER'),, wherein R and R represent hydrocarbon groups free from aliphatic unsaturation, E represents the ester linkage n is 2 or 3 and there are a total of 25 to 35 carbon atoms in the molecule,
b. 40 to 50 parts by weight of an alkylene oxide adduct nonionic surface-active emulsifier for fully emulsifying the ester oil in water, and
c. 0.5 to 5 parts by weight ofa water-soluble poly(oxyethylene-oxy-l ,2-propylene) glycol in which there are 1 to 3 parts by weight of oxyethylene groups for each part by weight of oxypropylene group and which has a viscosity of 5,000 to 50,000 Saybolt Universal Secondsat 100F.
A preferred ester oil lubricant is di(tridecyl)-adiapte. Others which are particularly suitable include di(undecyl)phthalate, di(n-decyDphthalate, trimethylolpropane tripelargonate, and di(tridecyl)phthalate.
A preferred nonionic emulsifier for the ester oil is about 40 parts by weight of tetraoleate'laurate of a reaction product of one mole of sorbitol with about 30 moles of ethylene oxide and about 5 parts by weight of a reaction product of one mole of nonylphenol with about 5 to 6 moles of ethylene oxide. However, a vari ety of suitable nonionic emulsifiers is known in the art.
The amount and viscosity of the poly(oxyethyleneoxy-l,2-propylene) glycol has been found to be surprisingly critical for satisfactory draw-texturing performance. If either is too low, then broken filaments result. It either is too high, twist-slippage causes nonuniformities in the textured yarn. Preferably, the finish composition contains 0.6 to 2 percent of poly(oxyethylene-oxy l,2-propylene) glycol which preferably has a viscosity of about 9,000 SUS at 100F.
The finish composition is particularly effective on incompletely drawn polyethylene terephthalate feed yarn for draw-texturing, but it is also useful on any of the synthetic textile yarns, including fully drawn yarn.
DESCRIPTION OF THE PREFERRED EMBODIMENTS The new finish, although being suitable for textile processing in general, is particularly suitable for processes in which textile yarns are heat-treated and make frictional contact with metal surfaces at high speed. It is particularly suitable for yarns which are feed yarns for a draw-texturing process. Partially drawn yarns have been used as feed yarns for the draw-texturing process. A more recent development is the use of yarns which are melt-extruded and pulled from the spinneret at very high speeds; e.g., of the order of about 3,500 yards/minute (3,200 m/min.). Such a process is described in Belgian Pat. No. 787,882. The yarns are so highly oriented that they need to be drawn only about 1.5 or 1.7X in the texturing process in order to develop adequate tensile properties and make them suitable for textile use. When used in conjunction with such yarns in the draw-texturing process, the new finishes show extremely little tendency to smoke, fume and form insoluble deposits on machinery and the new finish imparts to the yarn just the right amount of surface friction to avoid broken filaments and to insure against twist slippage. Twist slippage" refers to the slipping of twisted yarn past the false-twisting device of a texturing machine. Such a phenomenon causes yarn nonuniformities which'lead to fabric defects such as bulk and dye irregularities. The new finish does not contrib' monobasic acids include aliphatic and alicyclic acids,
pelargonic acid being preferred, and aromatic acids such as benzoic acid. Suitable diols include aromatic, aliphatic and alicyclic diols, 1,6-hexane diol being preferred. Suitable triols include trimethylolpropane and trimethylolethane. The dior triester component of the finish ofthis invention ispreferably free of aliphatic unsaturation and must contain from 25 to 35 carbon atoms in its moleculejDi and triesters having aliphatic unsaturatiomwhen used as finish ingredients, leave undesirable varnish deposits on contact with hotmachinery. Unwanted varnish deposits increase as molecular weight of the ester increases and they become more of a problem when using esters which have more than about 35 carbon atoms in their molecules. It the esters contain less than 25 carbon atoms, excessive fuming and smoking is a problem in hot processes. The preferred ester for use in the finish of the present invention is selected from the group: di(undecyl)phthalate, di (n-decyl)phthalate, di- (tridecyl)-adipa'te, trimethylolpropane tripelargonate and ditridecylphthalate.
The nonionic emulsifier of this invention is an alkylene oxide adduct of an organic compound having an active hdyrogen atom. Useful emulsifiers also function as lubricants. Compounds suitable for use in preparing such adducts are fatty acids and fatty alcohols, preferably unsaturated, ahving 12 to 20 carbon atoms in their chains, polyhydric aliphatic alcohols and partial esters thereof, and alkyl phenols. Another class of suitable nonionic emulsifiers includes the partial fatty acid esters of polyolsor their ethylene oxide .adducts. As is known, ethylene oxide adducts have hydrophilic properties due to the ethylene oxide moiety, and when the other portion of the adduct is primarily hydrocarbon so as to provide a hydrophobic moiety, the compound can be expected to exhibit surface-active properties. In general, ethylene oxide adducts-containing a chain of at least about 10 carbon atoms and at least three ethylene oxide units are useful in the practice of this invention. Preferably, the surface-active adducts will contain at least about 10 ethylene oxide units in their mole cules, since such compounds provide a composition with a high propensity for resisting the accumulation of electrostatic charges in addition to improving the manner in which'the composition can wet the filaments. Preferred surface-active agents are the adducts of ethylene oxide with a partial ester of fatty acids having at least 12 carbon atoms with polyols containing 3 to 6 hydroxyl groups, and the products obtained by esterifying an adduct of ethylene oxide and a polyol having 3 to 6 hydroxyl groups with a fatty acid having 12 to 22 carbon atoms. These products may be partial or complete esters and will preferably contain 20 to 50 ethylene oxide units in their molecules. A particularly preferred member of this class of surfactants is the material prepared by reacting one mole of sorbitol with about 30 moles of ethylene oxide and esterifying the product with about moles of a 4:1 mixture of oleic and lauric acids, it is preferred to use a mixture of this surfactant with an alkylphenoxy polyoxyethylene ethanolwhich, preferably, is the product of about 5 or 6 moles of ethylene oxide with one mole of nonylphenol. The combination of small quantities of about 2 to 10% (percentages of finish ingredients herein are weight percentages based on the weight of non-aqueous finish ingredients), of this emulsifier with the sorbitol derivative surfactant performs excellently. Itis essential that the nonionic emulsifiers fully emulsify the ester component of the finish in water. The emulsifier should be stable under conditions of use,i.e., it should have little tendency to smoke and form insoluble deposits when the yarn carrying the finish contacts hot surfaces.
The poly(oxyethylene-oxy-l ,2-propylene) diol of the present invention can be prepared as shown in US. Pat. No. 2,425,845. Of the polyoxyalkylenes useful for this invention, the weight ratio of ethylene oxide groups, i.e., the groups CH Cl-l O-, to propylene oxide groups, i.e., the groups is between about3:l and 1:1 in order that the material remain fluid and water-soluble. It is important that the viscosity of the polyoxyalkylene diol be between 5,000 and 50,000 SUS at F.; preferably, its viscosity is about 9,000 SUS at 100F. If the viscosity is too low, broken filaments of the yarn carrying the finish result; whereas, if the viscosity is too high, unwanted twistslippage in the draw-texturing process occurs. It is also important that the finish contain not more than 5 percent, and preferably not more than 2 percent, of the diol component. If the finish contains more than about 5 percent, unwanted twist slippage occurs in the drawtexturing process; if the finish contains less than about 0.5 percent broken filaments occur in the drawtexturing process. Generally, if the viscosity of the diol is high, less is needed and vice versa. It was totally unexpected that such a small amount of this ingredient would result in a drastic change in texturing performance of the yarn coated with the finish and, equally surprising, that more than 5 percent of this ingredient causes draw-texturing problems.
In addition to the above essential ingredients, small amounts of other materials may be added to the com position; for example, bactericides, buffering agents, tints, antioxidants, and the like, can be employed as circumstances may require.
The new finish composition is preferably used as an aqueous emulsion in which the non-aqueous or solids content ranges from about l to 25 percent based on the total weight of the emulsion. Emulsion concentration is preferably from 10 to 15 percent. It has been found that especially with draw-texturing feed yarn, such as shown in the Example herein, that high emulsion concentrations, i.e., greater than 10 percent, are preferred to maintain uniform moisture content within the yarn packages during periods of short storage.
Application of the new finish to the yarn can be done by passing the yarn across the face of a rotating roll emersed in the emulsion. The concentration of the emulsion and the roll speed are such as to apply to the yarn from about 0.1 to 1.5 percent solids, i.e., nonaqueous ingredients, preferably about 0.2 to 1' percent solids, by weight, based on the total weight of the tinished yarn. Solids is measured by extracting the tinish from yarn using carbon tetrachloride and measuring the amount of finish in the carbon tetrachloride by standard analytical techniques, such as gravimetric or infrared absorption techniques.
The new finish can be applied prior to drawing, for example, following the convergenece of the quenched filaments below the spinneret. The finish may also be applied during drawing as in a draw bath, just after drawing, or at some other point in the process.
While the finish of this invention may be used on synthetic yarns, such as polyamides, polyolefins, and the like, they are particularly well-suited to the manufacture of polyesters and copolymers thereof. Any of the polyesters may be used, but poly(ethylene terephthalate) is preferred.
DEFINITIONS AND MEASUREMENTS Break elongation andtenacity are measured according to the ASTM designation D-2256-69 (incorporating editorial edition of Section 2 and renumbering of subsequent sections as done in Mar., 1971). It is defined as in Option 3.3 Elongation at Break of Section 3. The testing is performed on straight multifilament yarns which were conditioned by storing them at 65 percent relative humidity and 70F. (21.1C.) for 24 hours prior to testing. An Instron Tensile Testing Machine is used. The test sample is 5 inches (12.7 cm.) long, 3 turns/inch (per 2.54 cm.) twist is added, the cross-head speed is inches/minute (25.4 cm./min.), the rate of attenuation is 200 percent/minute, and the chart speed is 5 inches/min. (12.7 cm./min.). The tenacity is the maximum load in grams before the yarn breaks divided by the initial denier of the yarn.
Coefficient of interfilament friction is a measure of the ease with which filaments slip by each other. About 750 yards (about 690 meters) of yarn are wrapped around acylinder using a traverse with a helix angle of and a winding tension of about 10 grams. The cylinder is 2 inches (5.1 cm.) in diameter and 3 inches (7.6 cm.) long. A 12 inch (30.5 cm.) length of the same yarn is laid over the cylinder so that it rests on top of the wrapped yarn and is parallel to the turn thereof. A weight in grams equal to 0.04 times the denier of the overlaid yarn is attached to one end of the overlaid yarn and a strain gauge is attached to the other end. The cylinder is then rotated at least 180 at a peripheral speed of 0.0016 cm./sec., so that the strain gauge is under tension. The tension is recorded continuously. The coefficient of interfilament friction, f, is then calculated by the following equation which is derived from the well-known equation for the friction of a belt running over a cylinder:
where T is the average of at least recorded peak tension values, T is the tension provided by the weight attached to the yarn, in is the mathematical symbol for the natural logarithm and Tr is the constant 3.14159. Data on yarn samples in which permanent elongation occurs during testing are not used. All data are collected at 70C. I I
Relative Viscosity (RV) values of the polyesters used in the examples are given as a measure of the molecular weight. Relative viscosity (RV) is the ratio of the viscosity of a solution of 0.8-gm. of polymer dissolved at room temperature in 10 ml. of hexafluoroisopropanol containing 80 ppm H SO to the viscosity of the H 80 containing hexafluoroisopropanol itself, both measured at 25C. in a capillary viscometer and expressed in the same units.
interlace pin count, as defined herein, is the length of yarn in centimeters that passes by probe 18 of US. Pat. No. 3,290,932 before the probe is deflected about 1 mm. A force of 8 grams is required to deflect the probe.
The invention will be further illustrated by the following example which is not intended to be delimitative.
EXAMPLES Poly(ethylene terephthalate) of 22 RV containing about 0.27 weight percent of TiO delusterant is meltspun at 290C. from a spinneret having 34 round orifices each 20 mils (0.051 mm.) in diameter and 200 mils (5.17 mm.) in length. The freshly spun filaments are quenched in a forced flow of F. (21.lC.) air and passed to a pair of high-speed puller rolls rotating at 3,400 yarns/minute (3,109 meters/minute) situated approximately 20 feet (6.0 meters) below the spinneret, make an S wrap around these rolls and then pass through an interlace jet device supplied with room temperature air at 60 lbs/in. gauge pressure (4.22 kg./m. to produce an interlaced yarn having an interlace pin count of 32 inches cm.). The yarn is then wound up at conventional package-delivery tension. A finish is applied to the yarn by passing it in sliding contact with a cylindrical finish roll emersed in a finish emulsion, located prior to the puller rolls. The finish remaining on the yarn is 0.5 percent solids, by weight, based on the total weight of the finished yarn. The tinish is composed of 55.17 parts of ditridecyl adipate, 38.67 parts of a surfactant which is prepared by reacting one mole of sorbitol with about 30 moles of ethylene oxide and esterifying the product with about 5 moles of a 4:1 mixture of oleic and lauric acids, 5.56 parts of alkylphenoxy polyoxyethylene ethanol which is the product of about 5 or 6 moles of ethylene oxide with one mole of nonylphenol, and 0.6-part of a poly(oxyethylene-oxy-1,2-propylene) glycol having a viscosity of 9150 SUS at F. The yarn has a relative viscosity of 22, a break elongation of percent, a coefficient ofinterfilament friction of 0.31, a tenacity of 2.3 gm./den., and a denier of 245.
The yarn is simultaneously drawn and false-twist textured on an ARCT-480 machine, commerically available from Ateliers Roannais de Constructions Textiles. The machine is designed to enable drawing simultaneous with false-twist texturing. In the texturing process, the yarn is fed from a package by feed rolls (first rolls) and passes upward through a heater tube to a false-twist spindle. It is pulled away by upper rolls (second rolls) driven at a higher speed than the feed rolls to draw the yarn. This increase in speed is accomplished by appropriate selection of gears. The heater plate in the twist zone is at a conventional temperature of 210C., the spindle speed is about 391,000 turns/- min. to produce in the yarn 60 turns per inch (23.6 turns/cm.) at a yarn speed of about 181 yds./min. m./min.). In this instance, the cooling zone which follows the heater plate is not used. The yarn passes from the upper rolls to a 230C. top heater at an overfeed of about 12 percent to a third set of rolls; the yarn passes to a fourth set of rolls at an overfeed of 4 percent and then to a package at a packaging overfeed of 2 percent. The draw ratio in the texturing zone is 1.5 8X. The textured yarn product is evaluated by counting the broken filaments protruding from both side walls of the package, a procedure commonly used in the trade.
During the process, essentially no fuming or smoking of the finish is noted and essentially no twist slippage occurs. The metal surfaces remain essentially free of varnish deposits. Broken filament count is shown in Table I. This yarn is identified as Yarn A.
The Example is repeated in all respects with the exception that 1.2 parts of the poly(oxyethylene-oxy-l ,2- propylene) glycol are used instead of 0.6. This yarn is identified as Yarn B.
The Example is repeated again in all respects with the exception that 0.3 parts of the poly(oxyethylene-oxy- 1,2-propylene) glycol are used instead of 0.6. The yarn is identified as Yarn C.
The Example is again repeated with the exception that the diol is omitted from the finish. This yarn is identified as Yarn D.
Table I indicates the broken filament count of these yarns.
TABLE I Poly(oxyethylene-oxypropylene) Yarn Glycol Level in Finish Broken Filament Count A 0.6 parts 0.3 B 1.2 parts 05 C 0.3 parts L8 D parts 2.5
' Number of broken filaments/pound.
It is seen that textured yarns which had been treated with finish containing poly(oxyethylene-oxypropylene) glycol at levels of 0.6 and 1.2 had acceptable broken filament count; whereas, the yarn treated with finish containing no or only 0.3 parts of glycol had an unacceptable broken filament count.
1. A polyethylene terephthalate textile yarn having 0.2 to 1 percent by weight, based on the weight of the yarn of a finish composition consisting essentially of a. about 55 parts by weight of di(tridecyl)-adipate,
b. about 40 parts by weight of tetraoleatelaurate of a reaction product of one mole of sorbitol with about 30 moles ethylene oxide,
c. about 5 parts by weight of a reaction product of one mole of nonylphenol with'about 5 to 6 moles of ethylene oxide, and
d. about 0.6 to 2 parts by weight of poly(oxyethyleneoxy-l ,2-propylene) glycol in which there are about three oxyethylene groups for each oxypropylene group and which has a viscosity of about 9,000 SUS at F.