US3470095A - Aqueous textile treating emulsion - Google Patents

Description

United States Patent 3,470,095 AQUEOUS TEXTILE TREATING EMULSION Joseph John Pontelandolfo, Charlotte, NC, assignor to American Cyanamid Company, Stamford, Conn., a corporation of Maine No Drawing. Filed Feb. 1, 1966, Ser. No. 523,913 Int. Cl. D06m 13/20 US. Cl. 252-83 6 Claims ABSTRACT OF THE DISCLOSURE A textile treating composition comprising an aqueous emulsion of ('1) a triglyceride of higher fatty acids; (2) hydrogenated tallow fatty acid; (3) a mixed ester of glycerol, said mixed ester having from 1 to 2 lower acyl ester moieties, the remaining ester moieties being higher fatty acid moieties; and (4) an ethoxylated castor oil.

This invention relates to the production of textiles and related materials. The invention relates to a non-ionic textile finish and to the production therefrom of treated fibers, staple fibers, felts, threads, cords, yarns, pellicles, filaments, fabrics and the like of synthetic or natural origin, or blends thereof. The textile finish is designed particularly for cellulosic textile materials, and blends thereof. More particularly, this invention relates to textile finishing compositions which impart softness to fibers, yarns and fabrics but which do not cause the fibers, yarns and fabrics treated with the composition to scorch when subjected to elevated temperatures.

The cationic textile softeners suffer from several disadvantages. Many of the cationic softeners are waxy or gummy in nature making them difficult to weigh or measure, to mix or disperse with other textile treating agents, and to place in a form, such as an aqueous dispersion, which may be readily applied to textiles. For these reasons, it is desirable to have a non-ionic softening composition capable of being effectively emulsified, having a high degree of storage stability, and capable of imparting both a softness of hand and a high degree of lubricity to the material being treated.

Softness is very frequently required in textile materials, particularly in fabrics used for clothing. The natural waxy, oily or fatty protective coatings of native fibers are often removed during the process of scouring and bleaching of these fibers. The fibers generally become harsh when these lubricants are removed, and fabrics formed from these fibers display an undesirable hand. In addition, certain coloring matters are prone to impart a dryness and an unpleasantness of hand to the fabric. Frequently, softeners are applied to fibers themselves to aid in the mechanical handling of these fibers since it iS very difficult to spin any fiber from which the natural oils or waxes have been removed or, as in the case of man-made fibers, those which do not contain a natural lubricant. Frequently, however, these treatments result in the production of a relatively stiff fabric which is harsh to the feel and less desirable commercially than fabrics possessing a soft hand. As a result, the industry has resorted to the use of several types of compounds for softening of finished fabrics and, in the case of rayon textile materials, for imparting thereto increased lubricity. The situations with which this invention is particularly concerned are those in which softeners are applied to yarn or fabric as a finish in themselves, to impart softness, smoothness, lubricity, fullness, suppleness, flexibility, and in some cases sewability as well.

There are a great many preparations available for softening textile materials and most, if not all, of these preparations are based on long-chain fatty or waxy comice pounds. The water-soluble soaps appear in a great many of these preparations, often for their softening properties as well as for their emulsifying properties. However, fabrics which include these soaps, which are soap-fat emulsions at their normal alkaline pH, exhibit a tendency to scorch when heated to the elevated temperatures encountered in certain textile processing operations. This tendency to scorch is apparently attributable to the presence of the soap or soap-like material. At the elevated temperatures encountered, the textile softening compositions containing fats or soaps become discolored or scorched, thus marring the appearance of the fabric. Among compounds heretofore used have been the sulfonated hydrocarbons, waxes, stearates, and sulfonated oils, such as cottonseed oil, peanut oil, coconut oil and similar oil products. Additionally, in view of the competitive economics involved in the textile manufacturing field, some of the most widely employed softening agents have been sulfated or sulfonated tallow, and sulfated or sulfonated monoand diglycerides of tallow, cottonseed oil, coconut oil, peanut oil and other compounds containing the relatively long carbon chain of the higher fatty acids. The presence of these materials even in small amounts in cotton and rayon textiles has resulted in undesirable yellowing of the fabric subsequent to heating thereof.

, Textile manufacturers do not find it economically expedient to treat only a portion of a particular lot of fabric for the scorch resistant textile finish. Furthermore, it is not known by the manufacturers how much or what part of a particular lot of fabric is to be subjected to elevated temperatures. Thus, it is desirable to have a heretofore unavailable composition capable of adequately being emulsified and capable of producing a softness of hand without the accompanying problems of being subject to scorching.

It should be noted that the adaptability of fibers, staple fibers, felts, cords, threads, yarns, pellicles, filaments, fibers, and the like to automatic handling operations is of extreme importance in the manufacture of textiles. Modern high speed machinery techniques require a feed of appropriate characteristics to permit uninterrupted and smooth operation. Accordingly, lubricity, softness, electrostatic qualities, and the like, of the material being processed are intimately related to the performance of the automatic mechanisms. Furthermore, the condition of the feed when it is subjected to the machine operations is likewise related to the excellence of the final product. For example, in the knitting industry, an improperly or poorly lubricated yarn produces uneven stitches. In the spinning of yarn, a minimal amount of lubrication is essential to the production of an even yarn, free of slubs. The problem is acute in the use of the more modern machinery, such as those employing the toe-to-top spinning process.

It is therefore an object of this invention to provide a textile softening composition suitable for use as a finish and characterized by a high degree of scorch resistance.

It is a further object of this invention to render scorch resistant, those textile softening finishes which norm-ally display a tendency to scorch.

It is a further object to obtain a textile softening composition characterized by non-ionic components having excellent emulsion characteristics, having a high degree of fluidity, having a high degree of affinity for textile materials, and being readily dispersible with other textile treating agents.

It is also a primary object of this invention to provide specially treated fibers, staple fibers, felt, cords, threads, yarns, pellicles, filaments, fabrics, and the like for the use in textile and related manufacture which possess combined characteristics of softness, lubricity, and anti-static 3 properties which render them especially adaptable to machine handling.

An additional object is to obtain a process for making the composition of this invention.

It is a further object to provide a process for treating these textile materials with the composition of this invention.

In accordance with the present invention, it has been discovered that the objects of this invention are obtained by the treating of textile fibers, staple fibers, felt, cords, threads, yarns, pellicles, filaments, fabrics, and the like, so as to coat or to impregnate them with a composition of matter comprising .(1) a glyceryl ester of a fatty-acid ranging from about 9% up to about 50%, (2) a hydrogenated member selected from the group consisting of the higher saturated and unsaturated tallow fatty-acids ranging from (zero) up to about 12%, (3) a lower acyl glyceride of a higher fatty-acid ranging from about 14% up to about 55%, and (4) a vegetable oil ethoxylated with from about 28 moles to 45 moles of ethylene oxide per mole of said vegetable oil, said ethoxylated oil ranging from about 14% up to about 75%, said percentages being based on substantially dry weight of said composition. The textile material treated with the above described composition results in a material which is highly adaptable to machine operations, combining the characteristics of softness, lubricity, and anti-static properties. The treated textile material is substantially non-wetting.

As noted above, the finishing compositions of this invention may be stored and shipped in a substantially anhydrous condition, or may alternatively be emulsified prior to shipping and storage by the addition of water in an amount suflicient to emulsify, normally about 20% or more. Subsequent to receipt of the finishing composition by the textile treating manufacturer, additional water may be added to the composition sufficient to prepare a dilution having the characteristics which might be preferred for the particular material to be treated.

Accordingly, the aqueous composition of the above finishing material contains water ranging from about 20% to about 83%, glyceryl ester ranging from about 4% to about 11%, the hydrogenated member ranging from 0 to about 2% (preferably about 0.1% up to about 1.5% the glyceride ranging from about to about 12%, and the ethoxylated oil ranging from about 6% to about 30%, where the percentages are based on the weight of the total aqueous composition.

It has been additionally found that the ethoxylated vegetable oil (such as castor oil) may be effectively supplemented by the presence of a polyalkylene glycol ester ranging from an amount suflicient to be effective up to about 2% of the aqueous composition, normally from about 0.1% up to about 1.5 to obtain the textile material of hand superior to that heretofore obtainable. The preferred polyalkylene glycol ester includes polyethylene glycol (1000) monostearate as at least a major component of the polyethylene glycol esters employed.

The glycerol esters of the fatty acid which may be employed include compounds of substantially similar structure such as glyceryl tristearate, glyceryl trilaurate, glyceryl trimyristate, glyceryl oleate, glyceryl palrnitate, glyceryl heptanoate, glyceryl caprylate, and the like. The glyceryl ester of the fatty acid which obtains the superior and therefore the preferred results of this invention critically includes glyceryl tristearate as at least a major component of the glyceryl esters employed. Similarly, the hydrogenated member which obtains the preferred results critically includes stearic acid as at least a major component of the hydrogenated members employed, other typical hydrogenated members including acids such as lauric acid, myristic acid, oleic acid, and the like. It should be noted, however, that superior results can be expected from the saturated fatty acids. Although the aceto glycerides are critical to obtain the preferred results of this invention, it is additionally within the scope 4 of the invention to employ other lower acyl glycerides of a higher fatty acid such as formoglycerides of the higher fatty acid. It should be noted that one of the more critical components of this invention is the vegetable oil ethoxylated with from about 28 moles to 45 moles of ethylene oxide per mole of the vegetable oil. The preferred results are obtained when the vegetable oil is castor oil. However, less effective substitutes therefor include ethoxylated peanut oil, ethoxylated coconut oil, and the like.

The preferred finishing composition which obtains superior results employs a vegetable oil ethoxylated with from about 35 moles to about 41 moles of ethylene oxide.

Additionally, it should be noted that the above described lower acyl glyceride of a higher fatty-acid is highly critical, in order to obtain the desired properties of the composition of this invention. The preferred results are obtained by the employment of a glyceride which includes glyceryl distearate-acetate as at least a major component of the glycerides employed. Other glycerides, less effective, however, typically include glyceryl stearate-diacetate.

For any of the above described components, the finishing composition of this invention may be used alone or in admixture with other substantially equivalent components of the type described above.

The preferred composition for application to textile materials includes glyceryl tristearate ranging from about 8% to about 10%, the stearic acid ranging from about 0.5% to about 1.5%, the glyceryl distearate-acetate ranging from about 6% to about 8%, the ethoxylated vegetable oil present in at least 8%, and the balance being water alone or in combination with another suitable solvent.

Both a characteristic of the finishing composition, as well as an advantage over prior compositions, is a low viscosity, characteristically a viscosity as low as about 19 centipoises at about 25% solids, and a very small particle size, substantially all particles being of a particle size below about 1 micron.

When the above composition is applied to textile material such as cotton, or a blend of cotton, or any of the other textile materials discussed above as within the scope of this invention, a new composition results, such as a textile material characterized by softness of hand and a lubricity discussed above.

Also, by the employment of the above composition as defined, a highly desirable and workable process for applying said composition to textile materials results from the highly emulsified composition in the aqueous solvent, which ordinarily is only water.

Also, by the employment of the above composition of this invention, the problems of poor stability have been substantially overcome.

It should be noted that an advantage of the composition of this invention lies in the ability to obtain a uniform softening of the yarn, as a result of the even distribution obtainable from the high quality emulsion of particles less than 1 micron in size. Another advantageous characteristic of the finishing composition of this invention is that it is highly soluble in either warm or cold water, thereby allowing it to be mixed at room temperature without bothersome, expensive, and time consuming heating up to obtain solution. The finishing composition resists both yellowing and odor development, and is nonchlorine retentive. Additionally, it is possible to have a high solids content which is characteristically higher than the normal solid content for a non-ionic liquid textile softener of this type, thereby resulting in a savings to the customer since the customer will be shipped more real product and less Water. Additionally, the product is very fluid, the viscosity thereby permitting easy pumping, metered measuring out of bulk storage, and no substantial change in viscosity Between temperatures of about 40 F. and F. The finishing composition of this invention is a non-ionic textile softener which can be used in thermosetting resin formulations, or as a pure finish to provide soft handle and lubrication to fabric or yarn which may thereby possess enhanced physical properties such as better draping qualities, better resistance to abrasion, reduced needle cutting, and the like.

The components of the finishing composition of this invention may be admixed in any conventional manner. However, to obtain the preferred composition, and to ascertain that composition has the preferred properties discussed above, it is critical to admix the components and to obtain a temperature of at least about 85 C., preferably at least about 89 C. for about 2 minutes to about an hour, preferably for about ten to about thirty minutes, followed by a prompt reduction of temperature to below about 30 (3., preferably below about 25 C. Thereafter the composition may be bottled and labelled.

A typical composition of this invention includes 8 parts of a glycerol ester of a fatty acid, one part of a hydrogenated member selected from the group consisting of the higher saturated and unsaturated tallow fatty acids, 8 parts of a lower acyl glyceride of a higher fatty acid, 8 parts of a vegetable oil ethoxylated with from about 28 moles to about 45 moles of ethylene oxide per mole of vegetable oil, and about 75 parts of water.

Another typical composition includes the components as set forth in the preceding paragraph, except that the ethoxylated vegetable oil emulsifier is present in about 6 parts, and the composition additionally includes about 2 parts of a polyalkylene glycol ester such as polyethylene glycol (1000) monostearate.

It should be noted that the aqueous composition employed in the process of treating a textile material rarely would contain more than 40% solids because solids content above 40% exhibits increased viscosity to such an extent that the ratio of expensive emulsifier to the other components becomes too great for the product to remain commercially feasible.

The following examples serve only to illustrate the invention disclosed herein, and do not limit the scope of the invention except as limited in the appended claims.

EXAMPLE I The components are admixed in a vessel, and heated to 89 C. with agitation for about twenty minutes, after which the mixture is quickly cooled to about 25 C. The composition includes 8 parts of glyceryl tristearate, 4.2 parts of stearic acid, 3.8 parts of diethylene glycol monostearate, 8 parts of polyethylene glycol (1,000) monostearate, and 76 parts of water. The composition is illustrated in Table I. The product obtained is initially fluid but sets to a paste within a few days, thereby exhibiting a poor stability.

Further experiments along this line fail to give satisfactory results.

EXAMPLE II The method of admixing components is the same as that for Example I. The components employed are 7 parts of polyethylene glycol (1000) monostearate, 13 parts of acetoglyceride and 80 parts of water.

The example is repeated employing acetoglyceride made from filtered tallow. Each of the above composi tions are given an application evaluation on fabric and the results indicate that each had improved hand, scorch and yellowing characteristics as compared to a standard conventional softener, but each of the above compositions set-up when placed in storage thereby demonstrating poor stability.

EXAMPLE III The composition is admixed according to the procedure of Example I. The composition includes 8 parts of glyceryl tristearate, 2 parts of stearic acid, 8 parts of acetoglyceride, and as emulsifier polyethyleneoxy ethanol in varying parts, the balance being water. An emulsion is not obtainable, demonstrating that the particular emulsifier is critical to the composition.

6 EXAMPLE IV Part A.The composition components are admixed by the process described in Example I. The components include 6 parts of glyceryl tristearate, 1 part of stearic acid, 10 parts of glyceryl distearate-acetate, 8 parts of ethoxylated castor oil, and the balance of water. The composition has a good appearance, and is illustrated in Table I below. The composition, employing 6 parts of glyceryl tristearate and 10 parts of glyceryl distearateacetate, illustrates that an acceptable composition of this invention may be prepared employing as low as the 6 parts of the glyceryl ester of the fatty-acid, and illustrates that 10 parts of the lower acyl glyceride of a higher fattyacid may be employed to obtain a satisfactory composition.

Part B.The composition of this invention is admixed according to Part A, except 4 parts of glyceryl tristearate is employed, and 12 parts of glyceryl distearate-acetate is employed. The composition is viscous, thereby demonstrating the lower limit of parts that can be employed of a glyceryl ester of a fatty-acid, and demonstrating the upper limit of 12 parts of a lower acyl glyceride of a higher fatty-acid.

EXAMPLE V The components are admixed according to Example I. The components include 11 parts of glyceryl tristearate, 1 part of stearic acid, 5 parts of glyceryl distearate-acetate, 8 parts of ethoxylated castor oil, and the balance of water. The composition has a very good appearance and is illustrated in Table I below. This composition demonstrates that 11 parts or more of a glyceryl ester of a fatty-acid may be employed to obtain a satisfactory composition of this invention. The example also illustrates the successful employment of as low as 5 parts of a lower acyl glyceride of a higher fatty-acid.

EXAMPLE v1 The composition is admixed according to Example 1. The components of the composition include 8 parts of glyceryl tristearate, 2 parts of stearic acid, 7 parts of glyceryl distearate-acetate, 8 parts of ethoxylated castor oil, and the remainder of water. The composition having good characteristics result, and is illustrated in Table I below. The composition of this example illustrates the upper limit of the amount of hydrogenated members selected from the group consisting of the higher saturated and unsaturated tallow fatty-acid which may be present.

EXAMPLE VII Part A.The components of the composition are admixed according to Example I. The components include 8 parts of glyceryl tristearate, 3 parts of stearic acid, 6 parts of glyceryl distearate-acetate, 8 parts of ethoxylated castor oil and the remainder of water. The composition so prepared is a paste and is accordingly unsatisfactory for the conventional treatment of a textile material, thereby demonstrating that 3 parts of the hydrogenated member exceed the maximum number of permissible parts, if an acceptable composition of this invention is to be obtained.

Part B.The composition is admixed according to Example I. The components include 8 parts of glyceryl tristearate, 4 parts of stearic acid, 5 parts of glyceryl distearate-acetate, 8 parts of ethoxylated castor oil, and the remainder of water. The composition thereby prepared sets, thereby illustrating an unacceptable composition, employing the hydrogenated number in excess of the maximum allowable for purposes of this invention.

EXAMPLE VIH Part A.The composition is admixed according to Example I. The components include 11 parts of glyceryl tristearate, 6 parts of glyceryl distearate-acetate, 8 parts of ethoxylated castor oil, and the remainder of water. The composition resulting was good, and is illustrated in Table 3,470,095 7 8 I below. This composition demonstrates that the comtrating this invention are intended to limit the invention position of this invention need not necessarily include a only insofar as stated in this specification and as the folhydrogenated member selected from the group consisting lowing claims are limited. of the higher saturated and unsaturated fatty-acids. I claim:

Part B.The composition is admixed according to 5 1. A textile treating composition consisting essentially Example I. The components include 9 parts of glyceryl of an aqueous emulsion of (1) from about 4 to 11% of tristearate, 8 parts of glyceryl distearate-acetate, 8 parts a triglyceride of higher fatty acids; (2) from about to of ethoxylated castor oil, and the remainder of water. 2% of a hydrogenated tallow fatty acid; (3) from about The composition is very excellent and further demonto 12% of a mixed tri ester of glycerol, said mixed ester strates the composition of this invention in the absence having from 1 to 2 acetyl ester moieties, the remaining of a hydrogenated member selected from the group conester moieties being higher fatty acid moieties; (4) from sisting of the higher saturated and unsaturated tallow about 6 to 30% of an ethoxylated castor oil, ethoxylated fatty-acid, as well as illustrating the use of a smaller with from about 28 to 45 mols of ethylene oxide per mol amount of glyceryl tristearate than was employed in Part of castor oil; and (5) from about 20 to 83% water said A of this example, Part A employing the maximum of percentages being based on the Weight of the total compermissible glyceryl ester of the fatty-acid. position.

EXAMPLE IX 2. A compositionaccording to claim 1, in which said ethoxylated castor oil 1s present in an amount of at least Part A.--The components were admixed in the manner about 8% by weight, said triglyceride comprises glyceryl described in Example I. The components include 10 parts t i t t present f about 3% t about 10% b 0f gly ryl tristeafate, 8 Parts Of g y ry distearate-aceweight, said hydrogenated member comprises stearic acid tale, 7 Parts of lf q P f the remainder present from about 0.5% to about 1.5% by weight, said of W The COmPOSItIOII 0f U11S lllvfilltlon thereby P mixed ester comprises glyceryl distearate-acetate present duced is excellent, and demonstrates the employment of from b t 6% t b t 8% by weight, aid a t oil a higher am of g y y ester of a fattv-aid,the1ack is ethoxylated with from about 35 to about 41 moles of Of y hydrogenated member of a Saturated or unsatur' ethylene oxide, said water is present in an amount of at rated a yt 3 Sma11er amunt of ethoxylated least about 57% by weight, and said composition is noncastor 011 than used in the foregoing examples. i0ni Part B.The components of the composition are ad- A composition according to claim 1, including a mixed according to the method described in Example I. The components include 10 parts of glyceryl tristearate, 1 part of stearic acid, 5 parts of glyceryl distearate-acetate, 9 parts of ethoxylated castor oil, and the remainder of water. The composition product of this invention thereby produced is excellent and demonstrates the employment of the lower limit of the amount of a lower acyl glyceride of a higher fatty-acid which may be employed and also Process treatmg teiftlle l compnsmg illustrates the employment of a higher amount of ethoxylapplylng a cfmlposltlon to a textlle materlal an amount ated castor oil than employed in any of the foregoing sufficient to 1mpart 3. softness Of hand and a degree polyethylene glycol monostearate ranging up to about 2% based on the weight of said aqueous composition.

4. A composition according to claim 1 having a viscosity of as low as at least about 19 centipoises at about 25% solids, and having individual particle sizes substantially all below about one micron.

examples, of lubricity to said material, said composition being de- Each of the above examples are illustrated in Table I fined according to claim 1. below: 6. A textile material characterized by a softness of TABLE I Parts per 100, by weight Example No 1 2 3 4A 4B 5 6 7A 7 B 8A 813 9A 9B Glyceryl tristearate 8 6 4 11 8 8 8 Stearic acid 4. 2 2 1 1 1 2 3 4 Glyceryl distearate-acetate 13 8 10 12 5 7 6 5 Ethoxylated castor oil--- 8 8 8 8 8 8 Water 76 80 var 75 75 75 75 75 75 Polyethylene glycol (1,000) monostearate-. 8 7 Polyethyleneoxyl ethanol (emulsifier) var. Diethylene, glycol monostearate 3.8 Appearance Poor Poor Poor Good Vrs. 00d pH l 4. 38 4. 40 4. 52 4.

No satisfactory emulsion possible. Viscous. Very good. Very excellent.

EXAMPLE X hand and a high degree of lubricity comprising a textile material having distributed thereon a composition ac- Employmg the general procedure of Example I, the cording to claim L composition of this invention is again prepared as follows:

The reactor vessel is charged with about 7500 lbs. of References cued water, after which about 900 lbs. of the emulsifier (such UNITED STATES PATENTS as ethoxylated castor oil) of this invention is charged, 2,005,785 6/1935 Hibb t r 1 252 3,6 X after which about 900 lbs. of hydrogenated tallow gly- 2,238,882 4/1941 Goodings et al. 2528.6 ceride (such as glyceryl tristearate) is charged, after 2,456,283 12/1948 J ff on 2528.9 X which about 100 lbs. of hydrogenated tallow fatty acid 2,978,408 4/1961 Lanner t 1 252 8,6 X is charged, and after which about 600 l s. of a g y- 3,039,895 6/1962 Yuk 2528.6 X cerides (such as glyceryl distearate acetate is g 3,170,876 2/1965 Olney 2528.9 X The agitator is run at highest speed and the r a t atch 3,198,732, 8/1965 Olney 2528.9 is heated to about 88-90 C., and is held at about 90 C. 3,306,850 2/1967 Olsen 2528.9 X for about 20 minutes, followed by cooling the batch to about 25 C. HERBERT B. GUYNN, Primary Examiner It is within the scope of this invention to make such modifications of the composition and process described above as would be obvious to a person of ordinary skill 117 139.5. in this art, and it is understood that the examples illus-