JPH0114346B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to hot melt sizing of textile warps, and more particularly to a new class of non-aqueous warp sizing applied to yarns in molten form. It has been recognized for several years that warp melt sizing systems have many benefits. Sizing Debate September 9-12, 1974 in Ptapest, Hungary [Melliand Textilberichte] English version 262
Page (Spring 1975)], regarding sizing machines and sizing, noted that ``If it were possible to use a sizing agent that cured at room temperature, all the problems with drying (energy prices, sources of error) could be avoided.'' It was done. Although there is currently no satisfactory, practical solution, melt size is likely to become important in the future. Prior to and since that time, progressive research in melt sizing and melt sizing methods and equipment has led to the development and patenting of numerous new size compositions. Nevertheless, various deficiencies, primarily the inherent economics, have limited the commercial acceptance of these sizes. U.S. Pat. No. 3,466,717 describes a warp sizing method and apparatus that applies the size in a sizing chamber with a butt containing a fast-setting melt size whose main component is wax. Examples of sizes applicable with this equipment are hydrogenated castor oil, 2-ethylhexyl acrylate and benzoyl peroxide, melt sizes made of one of the numerous sizes described in Japanese Patent Publication No. 40-14280. More broadly, the patent describes certain polymers or copolymers that dissolve in a special type of wax that can be applied to threads by a melt process. Three facts in this patent are of particular importance in connection with the present invention. First, it emphasizes the high compatibility of its various single or mixed polymer components with its wax components. Secondly,
If compatibility with Lowe is achieved, 2-
At least 20% of a hydrophobic vinyl monomer, such as ethylhexyl acrylate, must be present in the polymer component. Third, there must be a substantial portion of esters of hydroxycarboxylic acids, such as those found in hydrogenated castor oil or esters of hydroxy acids such as tartaric acid. The lowest 40% of this particular class of hydroxyester waxes is required as a component of the size composition described in the aforementioned Japanese patent specification. As a corollary of these facts, hydrogenated tallow is the best for the wax component itself, which acts as a solvent for the polymer component.
The specification of the Japanese Patent Publication emphasizes that it is 60%. More specifically, examples of the specification include 24
Size compositions containing more than % hydrogenated tallow are not shown. The Japanese Patent Publication does not foresee the use of a high proportion of readily available hydrogenated tallow in melt-sized compositions, ie, on the order of 50%. U.S. Pat. No. 4,136,069 discloses that melt-sized polymers prepared from polymer mixtures of high molecular weight and low molecular weight ethylene α,β-unsaturated carboxylic acid copolymers, such as mixtures of high molecular weight and low molecular weight ethylene/acrylic acid copolymers, is described. These molten mixtures are used alone or together with 0-50% of one or more <sub>C5</sub> - <sub>C12</sub> dicarboxylic acids, waxes, fatty acids or monoglycerides 0-30%, preferably 5-20% as the size. do. Regarding wax ingredients,
The patent does not mention animal or vegetable waxes. F. tropschii or primarily hydrocarbon waxes are the only species distinguishable by name and are shown as only minor substitutions in one example at the 2.5% level, as well as monoglycerides 17.5%. . It is an object of the present invention to provide a melt size that contains substantially more hydrogenated tallow or a significant amount of triglyceride tallow than previously permitted in a textile melt size. A further object of the invention is to provide a melt size that can be removed from textiles by extraction or washing methods with aqueous or organic solvents. A further object of the present invention is to provide a melt size with minimal smoke or gas generation during hot melt application to yarn. A further object of the present invention is to provide a melt size which imparts excellent weavability due to the increased abrasion resistance and fiber aging of the staple yarn to which the size is applied. These and other objects will become apparent from the following detailed description of the invention. The present invention involves melting approximately equal weights of fully hydrogenated tallow-type triglyceride wax with a special ethylene/acrylic acid copolymer to form superior fabric melt sizes. Optionally, the lower limit for copolymer content is about 1 to 7% hydrogenated tallow amide or other fatty acid amide.
The amount of tallow-type components may be increased by mixing up to about 35% by weight. Another embodiment of the invention incorporates from about 1 to about 9% sebacic acid or dodecanedioic acid into the mixture of copolymer and wax in varying proportions. Unlike the more complex melt sizing mixtures of the art, no very special polymer mixtures are required to obtain good sizing performance, or low contents of inexpensive hydrogenated triglyceride waxes. The unexpected benefits of the melts of the present invention are achieved without sacrificing performance or economic advantages. Hydrogenated tallow, preferably the preferred triglyceride wax of the present invention, has been known for a long time, and the art suggests that its significant advantages as a melt size component have been clearly recognized for many years. Nevertheless, the availability of simple, commercially available polymers and consistently high melt size ratios represents a surprising and commercially important advance in melt sizing of textile warp yarns. The hot melt size compositions of the present invention preferably consist essentially of 80/2 ethylene/acrylic acid.
0 copolymer and optionally 1 to 7% C <sub>16-20</sub> fatty acid amide or The copolymer content may be lowered to as low as about 35% by weight by incorporating 1 to 9% sebacic acid or dotecanedionic acid, and the copolymer is an ANSI/ASTM
When measured with condition D using D1238-79
It has a standard melt flow rate value of 250-550. Thus, in its broadest aspect, the melt sizing agents of the present invention contain <sub>C16</sub> to <sub>C20</sub> along with about 35-58% by weight of an ethylene/acrylic acid copolymer and about 62-42% by weight of a fully hydrogenated triglyceride such as hydrogenated tallow. It consists of a two- or three-component melt mixture of 0 to about 7% by weight of fatty acid amide and 0 to about 9% by weight of sebacic acid or dodecanedioic acid. For preferred binary sizes, we have shown that a composition range of about 45-55% by weight of substantially 80/20 ethylene/acrylic acid and about 55-45% by weight of hydrogenated triglycerides has shown the best results, with the highest Melt sizing properties are centered around a substantially 50:50 weight ratio of these components. A preferred triglyceride is tallow. In three-component embodiments of the invention, the content of ethylene/acrylic acid copolymer in the size may be as low as about 45% or as low as about 35% without significantly compromising the performance of the sized yarn. . The melt size of this embodiment is substantially ethylene/acrylic acid 80/20 polymer from about 35 to 45%, preferably from about 38 to 45%.
42%, about 62-54% hydrogenated triglycerides, preferably about 60-56%, and about 1% fatty acid amides.
~7%, preferably about 2-5%. It is believed that mixing the amide increases the mixing range of the copolymer and hydrogenated triglyceride, thereby allowing less copolymer to be used in the melt size. Compositions of the invention consisting of 40-55% ethylene/acrylic acid copolymer, 55-40% hydrogenated triglyceride wax and 1-9% sebacic acid or dodecanedioic acid exhibit an expanded range of melt compatibility; It can be melted and applied to threads at significantly lower temperatures than binary copolymer/tallow mixtures, ie, up to about 50% lower. Increased compatibility leads to intimate mixing with increasing temperature, and containing power at lower temperatures without separation of the melt components is advantageous. Mixtures containing sebacic acid or dodecanedioic acid have been shown to provide greatly improved smoke prevention at melt temperatures, and some of this prevention is believed to be due to the lower melt and application temperatures. They also appear to have increased thermal stability compared to mixtures of the invention that do not contain either acid. For maximum benefit from these property advantages, preferred compositions of this type are sebacic acid or dodecanedioic acid 4-7
% of copolymer and hydrogenated triglyceride in a ratio of approximately 50:50. Various other mixtures of sebacic acid and dodecanedioic acid may be used, always making up a total of 1 to 9%. The low molecular weight ethylene/acrylic acid copolymers used in the melt sizes of the present invention are well known and commercially available materials. They may be prepared by the methods disclosed in US Pat. Nos. 3,520,861 and 4,515,317, or smaller and preferably precipitated from the form of an emulsion as in US Pat. No. 3,436,363. The disclosures of these patents are incorporated herein by reference. Polymers in which the weight ratio of ethylene to acrylic acid is substantially 80/20 are best suited for the sizes of the present invention.
This type of commercial polymer has a composition and ANSI/
It is limited by both the melt viscosity shown herein as measured at condition D by ASTM test method D1238-79. This standard test
Polymers having melt flowability values of 250 to 550 g/10 minutes are useful in the present invention, with polymers having melt flowability values of about 300 being preferred. Hydrogenated or hardened tallow is a widely available by-product in the meat canning industry, which is produced primarily by the hydrogenation of beef tallow. As such it consists primarily of glyceryl stearate with small amounts of mixed glycerides of C <sub>14-20</sub> saturated fatty acids. Primarily because of its currently convenient price and availability, what is commonly known as fully hydrogenated beef tallow (iodine number less than 1) is the preferred triglyceride of the present invention. Other fully hydrogenated triglycerides, such as those derived from oils and fats such as soybean oil, cottonseed oil, peanut oil, palm oil, lard and tallow from sheep, goat and other animal sources, are attractive in the present invention. and they must be economically competitive. Kirk-Othmer's Encyclopedia
of Chemical Technology (Encyclopedia)
The table of composition of common plant and animal fats and oils in Volume 6, pages 142-144 (1951) of Chemical Technology) is helpful. It is noted that the majority of land-based plant and animal fats and oils have glycerides of their fatty acid components consisting of C <sub>14-18</sub> saturated and unsaturated acids accounting for 85-95%. When completely hydrogenated,
These acids are essentially converted to stearic, palmitic, and myristic acids, and the product triglycerides, which are essentially identical to fully hydrogenated tallow mixtures of these various waxes, can also be used. Expressly excluded from the triglyceride species of the present invention is castor wax, which is a fully hydrogenated derivative of castor oil. Due to the very high proportion of ricinoleic acid in castor oil, castor wax with a correspondingly high content of 12-hydroxystearic acid moieties is unsuitable for use as the main component of the melt size of the present invention. Fatty acid amides, also known commercially as hydrogenated tallow amides, are usually produced by the reaction of free acids or hydrogenated tallow with ammonia.
A representative mixture of C <sub>14-20</sub> acid amides, primarily stearylamide. More chemically specific fatty acid amides may of course be used in the present invention, but are usually more expensive. In addition to the listed ingredients, small amounts of other agents such as tracer dyes, antioxidants and the like may be added to the sizes of the invention if desired. Although other methods may be used as variations, the application of these sizes is
The method and apparatus of No. 29287 are preferred, and the contents of this reissue patent are incorporated herein by reference, and are useful in describing methods of using the melt-sized compositions of the present invention. Typically, a predetermined amount of hydrogenated tallow is melted by heating to near smoke temperature and the ethylene/acrylic acid copolymer is added sequentially with stirring to complete the mixing. Then,
The fatty acid amide or dicarboxylic acid, if used, is stirred in and the melt is then poured into a suitably sized pan or dish and cooled to a solid mass or size. Rapid cooling is desirable to minimize separation of components. As described in reissued patents, size blocks are typically
It is directed against and pressed into the groove of the applicator roll heated at 350-400㎓, and the size is taken out from the groove as a thread path along or along the arc of the rotating roll. The invention will be explained in more detail in the examples given later. Desizing agents can be conventional alkaline aqueous detergents or organic solvents, or our U.S. Pat.
4253840 (dated March 3, 1981) with a mixture of petroleum solvents and methanol. In our experience, in the field of melt sizing, the need for relatively high melt and application temperatures to ensure rapid size solidification on the yarn and prevent the tendency of hot sizes to gasify and smoke It has been found that there is a delicate balance between the need to avoid thickening or gelling on the applicator roll, or at least to bottom out. There used to be. Within the preferred application range of 350~400〓 for the size of the present invention, the sizing operation is smooth,
and the indicated upper limit is generally selected as long as it continues without periodic pauses for adjustments, thread cuts, and the like. At about 400〓, the size is less viscous than at 350〓 and flows more freely into the yarn. At high temperatures, the propensity for gasification and fuming is naturally greater, but is minimal and better than what we have observed for other high melt sizes within the entire temperature range. The lowest temperature of the preferred application temperature range greatly prevents gasification and fuming, and in particular significantly slows down the rate of thermally induced reactions that would otherwise lead to size gelation or other premature solidification at the application temperature. Thus, when starting, the applicator roll should be approx.
Heating to 350° is preferred; at other times unscheduled delays will cause the melt size to remain on the applicator roll longer than desired. The inventor believes that the unusually high content of hydrogenated tallow in the sizing agent is responsible for a non-negligible amount of the observed remarkable sizing performance. Although not intended to limit the scope of the invention except as limited by the claims, the inventors believe that a certain desired limit of incompatibility of the size components with each other is the basis of the advantages of the invention. Think about it. This incompatibility is particularly evident at the upper % level of tallow, ie, above about 55% tallow in the preferred two-component size. For the most part, conventional art teachings regarding melt sizing appear to insist on a high degree of compatibility of the melt components with each other. This is particularly clear in the above-mentioned Japanese Patent Publication No. 14280/1973. On the other hand, we devised a critical range of sizes in which the melts become miscible only near the application temperature, and then quickly revert to incompatibility as they cool and begin to set on the yarn. was successful. The compositional parameters of the present invention were achieved in terms of our melt size performance characteristics. Based on the inventors' observations and data, ethylene/acrylic acid copolymers having a melt flow rate value of 250 to 550 as described above have a relatively low compatibility of melt components. Seems excessive. In any event, the melt becomes so viscous that it can hardly be used as a melt size at this high percentage of polymer and above. In two-component melt systems, lowering the polymer content below about 40% by weight results in unsatisfactory compatibility in the melt and inconsistent and non-uniform sizing performance. The lowest limit of copolymer content may be expanded somewhat, i.e., about 35% by weight by mixing small amounts of fatty acid amides without disturbing the unstable balance of high tallow melts.
It may be expanded to The tallow acts as a dispersant for the polymer to a small extent at the application temperature, but as cooling sets in and if all the tallow remains in a single mixed phase upon cooling, the We believe that at higher polymer contents, sufficient phase separation occurs that the yarn is coated with a size film that has greater strength and flexibility than would be expected. An important advantage of the present invention in view of the limited compatibility of size components is that the size yarns are very well woven on a loom. It is uncommon to have no tendency to stick to and build up on the healds and other loom parts, especially in such high wax content sizes. This property, which we envision along with the lack of tackiness of yarns sized over a wider than normal temperature range, is much more pronounced in yarn sizing situations than mere measurements of size film strength and elongation. Perhaps because of their unusually high resistance to sticking, the sizes of the present invention can be successfully applied at higher coverage than most melt sizes without adversely affecting either sizing or weaving performance.
The above-mentioned Japanese Patent Publication states that, for example, in doubling, weaving, knitting, etc., if the amount of size applied exceeds 4% by weight, problems will occur. The sizes of the invention have been successfully applied to yarns of various types and sizes in amounts ranging from 8 to 18%. Less coverage can be applied to less demanding yarns than the hairy spun yarns most tested in the course of this invention. The loom performance is excellent. The following examples describe several tests that the inventors believe are simpler and faster than actual weaving. A number of these tests were used to evaluate and select candidate melt sizes for the present invention. ANSI/ASTM D1238-79 for melt size composition preparation for initial laboratory screening.
The indicated standard melt flow rate value measured in condition D by
A small sample of an ethylene/acrylic acid 80/20 copolymer having a compound (hereinafter abbreviated as SMFR) was melt mixed with a planned amount of hydrogenated tallow and tallow amide. Typically, for a 50/50 mixture, 30 g of copolymer was melted and 30 g of hydrogenated tallow was stirred into it, and the melt was observed to become clear at 400 g. The melt was then poured into a 0.5 x 0.75 x 7 inch Teflon mold and allowed to cool. Larger samples may be produced in essentially the same way. Bruckfield Viscosity Measurement - A simple measurement useful for sizing the present invention is the Bruckfield viscosity, more specifically, the continuous Burckfield (model LVE) viscosity measurement on the same melt. Calculated coefficient of variation
coefficient of variation) (COV). For this measurement, 10 g of the molded size rod was melted in a constant temperature bath and then heated at 400 rpm at 60 rpm using spindle No. 4.
Measure at 〓. Take 10 consecutive measurements and then analyze to determine the COV. The viscosity is moderately time dependent, as melts are known to gel if melted and held overnight, so measurements were taken as quickly as possible, approximately every 30 seconds. To preliminarily screen various size compositions for the threads, the ends of the molded size rods were placed against a six-groove laboratory mold of a melt applicator roll of the type described in U.S. Reissue No. 29287. The size was applied to the six threads by pressing. 400
〓The heated roll is rotated at 10 rpm in the direction in which the yarn moves.
during which the yarn, traveling at 330 yards per minute (ypm) unless otherwise indicated, passed through a groove at the neck of the roll. The tension applied to the sizing thread was measured using a conventional tensiometer. Abrasion Testing - As a screening method to evaluate the relative resistance of the sized yarns to abrasion in a shuttle loom, a rapid abrasion test was performed on the majority of the test samples. The device used consisted of a vertically fixed heddle attached to the neck of a short rod, which was successively tightened at the bottom of the rod to the shaft of a horizontally fixed air cylinder. The thrust of the cylinder is controlled to provide a horizontal reciprocating motion of 4 inches in each direction along a straight line to the heald. Secure a thread clamp and 1/8-inch rod above and parallel to the passageway of the cylinder shaft and approximately 1 inch below the bottom of the heald hole, with the clamp and rod extending 10 inches between them with the heddle hole. is seperated. To test, each yarn sample is secured in a clamp, passed through the heddles, and a 90 g weight attached to the rod is pulled to tension the yarn. Thus, at the midpoint of the 4-inch heddle stroke, the thread forms an isosceles triangle 1 inch high with the 10-inch line between the thread clamp and the hook. To better simulate the action of a loom, set the horizontal plane of the heddle stitch about 20 degrees from normal relative to the thread line, as you would set a heddle on a loom. The device operates at a speed of approximately 150 round trips/minute. A counter records the number of round trips. In abrasion devices such as those mentioned above, the 90 g weight applied to the yarn, typically to approximate the tension on the loom, makes the test very demanding. Each counted reciprocation or stroke of the heald consists of passing through and returning to the starting point. The operator monitors the yarn very carefully from the beginning of the test and records the counter reading when the quality of the yarn begins to deteriorate (unwanted sizes practically deteriorate quickly). If the number of strokes before cutting is desired, the device will continue to operate until the thread breaks. At least 20 samples of each yarn are typically tested to a "good yarn" average value in the range of 3.0 to 5.0. Strokes to break for such threads range from 200 to 250. If the coarse and hairy surface of the warp adjoining threads appears to cause internal warp friction and knots under the action of the loom, the formation of fluff beads will be extremely short. This indicates that the quality of the thread has deteriorated. A 90 g weight with an accompanying low but uncertain number of tests was retained for speed and efficiency in sorting out likely failures among a large number of samples. A good correlation was observed between relatively high ratings in the test and actual performance on commercial looms. Size Estimation - Another test to screen the likelihood of a melt size that can be successfully woven on a loom involves evaluating the tendency for size to estimate on the loom section. The device consists of a 1/8 x 12 inch stainless steel rod (bowed 6 inches and 0.5 inches up toward the center) mounted essentially horizontally on a reciprocating wooden platform, thereby allowing the The rod moves 4 inches in each direction along. A thermocouple is attached to the bottom of the rod at its center for the purpose of measuring the temperature change in the rod. On each side of the bar, parallel to it,
And install 0.5 inch aluminum rods 7 inches apart. Raise the center of the rod 1.5 inches above the horizontal plane of the two rods. On the outside of the bar and slightly below there are two beams for feeding and winding the test warp threads. To perform a full yarn test on this device, 90 melt-sized yarns are wound onto a beam to approximately 30 yards as warp yarns, and the warp yarns are fed across a stainless steel rod and a second rod to a first aluminum rod. , given by a brake weight suspended from a supply beam.
100~110g/1 piece of winding beam under tension
Lower through a 4.5 inch comb. The warp is approx.
Pull across the device at 10 yards/hour. The warp thread friction on the test bar is determined by recording the temperature of the bar, which is typically room temperature during effective size testing. to about 105〓, and rises to about 125〓 for marginal or bad sizes.
Other evidence of poor sizing performance is lateral or wavy action of the warp threads, sticking to the rod or pecking,
In that case, the exam usually ends early. When a given warp of 30 yards has been completely passed through, carefully examine the rod for any evidence of stickiness of the size and, if not, record it as ``no stickiness'' and the size is completely be considered as a candidate for the weaving test. If there is any loose dust on the wooden stand, record it in the notes as it indicates the possibility of dust scattering of the size on the loom. Melt Segregation - In addition to observing the turbidity of the melt at 400ⓓ as recorded here, another evaluation of the homogeneity of the melt was performed in some cases. This is because when the agitated melt is raised from the stirrer out of the melt and then lowered into the melt, fibrous material may be present in the melt.
It involves observing the approximate temperature that indicates the melt compatibility of the mixture, defined as the point at which it no longer shows evidence of lumps, swollen grains, or the like.
Below that temperature, the wax components tend to separate into a floating layer on top of the copolymer when stirring is stopped. It is also a property of this temperature point. Above this temperature the molten mixture, although still somewhat hazy in appearance, does not exhibit such separate component layers. The following examples relate to the above tests; all parts and percentages are by weight unless otherwise indicated. In the claims, the total weight percentages of the indicated ingredients are 100%. When present, certain components are present in an amount of at least 0.1% by weight. Example 1 Hydrogenated tallow and ethylene/acrylic acid 80/20
Equal amounts of (EAA) polymer were simultaneously melted. The Burtskfield viscosity for the size was 825-850 cps. Size coverage on polyester/cotton thread (65/35) 25/1 was 15.7% on a 400 〓 roll with a 1 inch groove, and the sizing operation was smooth for a long time. In the abrasion tester, the sized yarn showed a good record of 5.2 strokes before yarn quality deteriorated and 202 strokes before breaking. In the size deposition tester, the sized warp progressed a complete 30 yards, and the test bar was free of deposits after the test was completed. Example 2 Sizing was performed using the same 50/50 melt size method as in Example 1 except that the SMFR of the copolymer was 300 and the size coverage of the polyester/cotton thread was 19.2%, and the abrasion test results were It took 6.8 strokes until the thread quality deteriorated. The sized warp threads were evaluated as "no deposits" in the size deposition test. Example 3 A series of screening experiments were conducted using the EAA copolymer of SMFR 300 in melt mixtures with varying weight ratios of hydrogenated tallow according to the general method of Example 1. The results are shown in Table 1, sized and tested as detailed above and applied to polyester/cotton threads.

Table *Examples other than the invention These data show that the EAA/tallow ratio in the middle range results in essentially the same good performance results. However, at the high copolymer ratio of 60/40, two defects begin to appear. One is clear from the data, that the viscosity is higher than desired, indicating that during sizing, the yarn will be overly tensioned. Other flaws are somewhat less obvious. From these and similar experiments, we have learned that if the molten components appear too compatible, they are of a size outside the claimed scope of the invention. In the series of Table 1, the EAA/tallow 60/40 composition is the only one whose melt is completely clear at 400°C, the others are somewhat opaque or cloudy at this temperature. This observed turbidity appears to be evidence of marginal compatibility which apparently results in superior melt sizing performance. Concomitant with the high compatibility of the EAA/tallow melt is a lower than average coefficient of change in continuous Bruckfield viscosity measurements. EAA/tallow 40/60 mixtures at the top of the table (or other examples other than the present invention) have the opposite disadvantage, as exemplified by an excessive COV of 12.7. Such a high level of variation in continuous Brookfield viscosity measurements indicates a highly heterogeneous melt and poor miscibility of the components. Compared to other melts, this high proportion of tallow composition is not only excessively cloudy at 400 〓, but careful testing shows that the melt is clearly non-uniform and poorly dispersed. It was clear that there was visible evidence of the polymer. The data and observations indicate that for the two-component melts of the present invention, good sizing is achieved when the weight ratio of EAA to tallow is centered around a 50/50 ratio, and ranges from about 55/45 to 45/55. There is a sexual plateau. Example 4 In a further series of screening experiments, the EAA/tallow composition was tested by relying on a three-component composition.
It has been found that the lower limit of EAA content can be lowered somewhat, ie, by adding a smaller proportion of fatty acid amide, the mixing range indicated in the first part can be expanded. SMFR
The method of Example 1 was carried out using an EAA copolymer having an EAA of 300. A specified amount of molten hydrogenated tallow amide was added at a rate of about 400 ml with stirring, and size bars were manufactured as before. Table 2 shows the experimental results. For comparison, EAA/Tallow 40/
Add 60 results. Table 2 shows the results obtained with the copolymer content fixed at 40%.

[Table] * Examples other than the present invention These EAA40 containing hydrogenated tallow amide
% composition, the results clearly show that the problem of excessive incompatibility associated with the EAA/hydrogenated tallow sizes in Table 1 has been largely eliminated.
Throughout the range of these ternary compositions, the data are completely satisfactory and the incompatibilities, as measured by COV, are within the required range for melt size. The only limitations observed were a tendency towards excessive brittleness and powder scattering in compositions containing 6% and 8.4% hydrogenated tallow amide. Example 5 The range of compositions evaluated in Example 4 was expanded by lowering the EAA content to 35% and then to 30%. Table 3 shows the results.

[Table] *Example other than the present invention Content of ethylene/acrylic acid copolymer is 40%
It can be reduced to below, but below about 35%,
These data show that the COV clearly exhibits excessive incompatibility in the mixture. On top of that,
When the copolymer content is 30%, the size abrasion resistance is insufficient. Example 6 Polyester/cotton (65/35) 25/1 warp sizing was increased to commercial scale with 400 threads on a melt applicator roll with 600 grooves, roll temperature 350-360〓, roll speed 11.5 rpm and The blocks were sized at a feed rate of about 1 inch/minute. Yarn speed is 380ypm and size coverage is average approx.
It was 13%. The size was a 50/50 mixture of ethylene/acrylic acid 80/20 copolymer with an SMFR of 300 and hydrogenated tallow in the form of 7/8 inch blocks. The yarn was sized onto each of the 10 beams and wound onto the section beams until 3200 yards of yarn were obtained. The section beam is then re-wound onto two Sulzer loom beams, each holding 3992 warp threads. The beam was attached to a double warp Sartzer loom to weave a 120 inch fine cloth fabric. The weaving performance based on the loom efficiency of the number of warps was compared with the weaving of other conventional water-based sized warp yarns woven in the same style with the same weaving area. Hot-melt sized warp threads average only 46.3% of the number of loom stops associated with the warp threads of normal warp threads, and their loom efficiency is approximately 5% lower than that of normally sized warp threads.
% was high. Example 7 Ethylene/acrylic acid 80/2 with SMFR 300
A molten mixture of 45% copolymer 0, 48% hydrogenated tallow and 7% sebacic acid was prepared in the binary size of the invention at various ratios of copolymer and tallow.
The melt was heated until it became compatible as defined above at a temperature of about 280°, which is about 70° below the commonly observed temperature. The size was preliminarily selected by applying it to yarn as in Example 1 at a coating weight of 12.5%. The sized system performed well in the abrasion tester when compared to the two-component size of the present invention. Example 8 A similar melt mixture of 50% copolymer, 46% hydrogenated tallow and 4% sebacic acid was also compatible at about 280%. The most promising property observed with this melt was its surprising resistance to gelling upon prolonged heating. The Bruckfield viscosity of the melt held at 350°C was measured (spindle No. 4, 60rpm), and the starting viscosity was
1700cps after 24 hours 2350cps then 48 hours later
It only increased to 5000cps. Example 9 Another melt mixture consisting of 47.5% copolymer, 47% hydrogenated tallow, and 5.5% sebacic acid also contained about 280
〓 indicates compatibility. In the Bruckfield viscosity test of Example 8, the starting viscosity was 1200 cps in 24 hours.
1250cps, 2500cps in 48 hours and 90 hours
Although it increased by 5300 cps, it did not gel. It was hardly expected to have such a long resistance to thermal degradation compared to tests with similar compositions with lower amounts of dibasic acid. Example 10 A melt mixture of 32% copolymer, 59% hydrogenated tallow and 9% sebacic acid becomes compatible after some time at 300 ml, but the film cast from the melt is too small as the melt size. It was judged to be fragile and not useful. Example 11 A melt mixture of 47.5% copolymer, 47% hydrogenated tallow, and 5.5% dodecanedioic acid becomes compatible at 280% and exhibits resistance to gelation compared to the melts of Examples 8 and 9. Indicated. The initial Bruckfield viscosity of 1326 cps was changed in just 24 hours, except that under the conditions of Example 8 the melt temperature was 360°.
1598cps, 1748cps in 32 hours, and 56 hours
It rose to 2894cps. Samples made from 3.5 mil films cast from fresh melts of this composition on an Instron tester had tensile strength measurements of 954 psi and elongation at break of 430%, compared to the best size of the present invention. The price was comparable to that of the film. Although particularly suitable for sizing polyester/cotton, the melt sizing of the present invention is suitable for sizing other natural and synthetic yarns, such as 100% cotton, 100% wool,
Suitable for sizing wool/cotton, wool/polyester and other yarns. The invention may be embodied in other forms or carried out in other ways without departing from its spirit or nature. This embodiment is for illustrative purposes;
The scope of the invention is indicated by the claims, and equivalents are intended to be encompassed therein.

Claims (1)

[Claims] 1. From an intimate mixture of 42% to 58% by weight of a substantially 80/20 ethylene/acrylic acid copolymer and 58% to 42% by weight of hydrogenated tallow-type triglyceride wax. a textile melt size composition, wherein the size is applied as a melt to textile yarns, can be rapidly set when exposed to environmental conditions, and can be removed from the yarns by aqueous or alkaline extraction. A rapidly fixing non-aqueous water-extractable textile melt size composition capable of fast fixing. 2. The melt size composition of claim 1, wherein the ratio of copolymer to tallow triglyceride wax is about 50:50. 3. The melt-sized composition of claim 1 or 2, wherein the copolymer has a standard melt fluidity value of 250 to 550 when measured in condition D according to ANSI/ASTM D1238-79. 4 35% to 58% by weight of substantially 80/20 ethylene/acrylic acid copolymer, 62% to 42% by weight of hydrogenated tallow-type triglyceride wax, and up to 9% by weight of sebacic acid or dodecanedioic acid. a textile melt size composition consisting of an intimate mixture with a textile yarn, the size being applied as a melt to textile yarns and capable of rapidly fixing when exposed to environmental conditions, and having aqueous or alkaline extraction A fast-fixing non-aqueous water-extractable textile melt size composition that can be removed from yarn by. 5 The amount of copolymer is 38% to 42% by weight, and the amount of tallow triglyceride wax is 56% to 42% by weight.
60% by weight and the amount of sebacic acid or dodecanedioic acid is from 2% to 5% by weight. 6 In close contact with 35% to 58% by weight of substantially 80/20 ethylene/acrylic acid copolymer, 62% to 42% by weight of hydrogenated tallow-type triglyceride wax, and up to 7% by weight of fatty acid amide. A textile melt size composition comprising a mixture, the size being applied as a melt to textile yarns, capable of rapidly setting when exposed to environmental conditions, and being removed from the yarns by aqueous or alkaline extraction. A fast-fixing non-aqueous water-extractable textile melt-sized composition that can be used. 7 The amount of copolymer is from about 38% to 42% by weight, the amount of wax is from about 56% to 60% by weight, and the amount of amide is from about 2% to 5% by weight.
A melt-sized composition according to claim 6, wherein the melt size composition is up to % by weight.