Juan
Patented Aug. 11, 1953.
UNITED STATES PATENT OFFICE Gergxzi j il ift fj i izgz g fia assignor to American Viscoseflorporation, Wilmington, Del-., a corporation" of Delaware No Drawing. Ap iidatimj yo ember 19,1947, Serial No. 787,023"
30laims. (o1. 166L165)" This-invention relates to fibers and yarns com-- prising regenerated cellulose characterized by high breaking toughness and low average"stifi-- ness, and to the production of such fibers and yarns from viscose;
Breaking toughness is defined as the work required to break a given yarn, and has the dimensions gram centimeters per denier centimeter. It is numerically equal to the area under the stress-strain curve obtained from various tensile strength testing machines. Average stiffness is a measure of the extensibility of the yarns at a given load and is numerically equal to the ratio of-thetensile strength at break, to the elongation at break. The terms breaking toughness and average stiffness are explained in detail in the paper by Harold De Witt Smith, published in the Proceedings of the American Society for Testing Materials, vol. 44, 1944, pp. 589-90.
In the past, the production of fibers and yarns from viscose having the combined characteristics of high breaking toughness, and low average'stiffness, has invariably involved changes in' the composition and salt test of the Viscose, as Well as in the spinning conditions, as compared to the Viscoses and spinning conditions normally used 'for'the. production of fibers and yarns.
The object of the present invention is to produce fibers and yarns characterized by high' breaking toughness and low average stiffness from conventional viscoses having normal so- -dium hydroxide and cellulose content, of normal sa1t point (as determined by the standard sodium obtained from a normal viscose of the same sodium hydroxide and cellulose content and salt point, and under the same spinning conditions, but in the absence of urea admixed withthevis cose.
The effective amounts of urea are in the range of from about 1 to 5%, based on the weight of the viscose.
Any normal viscose may be'used. Such normal- 'viscose" have a sodium hydroxide content of from 6 to '8%,-based'on thewei'ght of the viscose, cellulose contentof from 6 to 8%, based on the weightof the viscose, and salt points in the range or frame to 6.
The mixture comprisingviscose and from about 1' to5%' of urea by weight may be spun into adueo'u's' acid spinning baths containing from about8 to'l2% sulfuric acid, from about 2 to 5% zinc sulfate, and from about 16 to 20% sodium sulfate; the baths being maintained at normal temperatures of from about 55 C.
In all instances, the ureaexerts a marked effect upon the breaking toughness and average stiffness' 'o'f the fibers and yarns obtained. However, in generaLthe effects of'the urea are more noticeable in the case'of viscoses having the lower salt points in the range of 3 to 6 stated. The lower the'saltpoint (i. e. the more highly ripene'd or aged the viscose) the greater the increase in the breaking toughness, and the greater the decrease in average stifiness of the fibers an'd yarnsobtained, v i
The urea may be added at any stage in the course of the viscose production, but preferably the1ur'eais admixed with the viscose immediately after its p'roduction and prior to storage thereof for ripening', during storage of the viscose for ripening," on after the viscose has been ripened and immediately prior to spinning the fibers or yarns. The urea does not substantially efi'ect the saltpoint' of the viscose, or the processes which normally take place during ripening thereof.
The following specific examples will serve to illustrate the invention. In carrying out the processes of the'examples, the stress-strain curve mentioned bySmith' (supra) was obtained by means of theScottinclined plane tensile strength testing machine which is described in detail in the'arti'cleby'A. Stuart Hunter, entitled Importanceof Uniformity in the Constant Rate of Loading'iwith the Scott Inclined Plane Serigraph, American'isilkand Rayon Journal, January 1937.
Example 1 About2.5% of ureawas added, with stirring, to arviscosecontaining'about 7.8% sodium hydroxide'andr'about' 7.5% of cellulose, by weight,-'
denier yarn wh'ich 'was 'g-iven a godet stretch of 1 Qn testing," the yarn was found to have a dry breaking toughness of"51.9 gJcm/d. cm. and
average stiffness of 23.2, wet breaking toughness of 28 g. cm./d. cm. and wet average stiffness of 13.6. This compared with a dry breaking toughness of only 38.8 g. cm./d. cm. and average stiflness of 27.2; wet breaking toughness of 20.9 g. -cm./ d. cm., and wet average stiffness of 21.5 for a yarn spun from a viscose of the same composition, under the same conditions, but which did not contain urea.
Emample 2 To a viscose containing 7.8% sodium hydroxide and 7.5% cellulose, and having a salt point of 5.9, there was added 1.25% of, urea by weight. The viscose was then spun into an aqueous bath containing about 11% sulfuric acid, about zinc sulfate, and about sodium sulfate, to produce a 150 denier, filament yarn, which was given a godet stretch of about 69%. The yarn was after-treated in the usual manner, and dried, after which it was tested for breaking toughness and average stiffness. It was found to have a dry breaking toughness of 51.8 g. cm./d. cm., and average stiffnes of 17.0; wet breaking toughness of 37.7 g. cm./d. cm., and wet average stiffness of 9.5. A similar yarn, produced from a viscose of the same salt point and basic composition, but not containing urea, was found to have a dry breaking toughness of only 47.8 g.
cm./d, cm. and average stiffness of 18.7, and wet breaking toughness of 32.3 g. cm./d. cm. and average stiffness of 9.9.
Example 3 About 2.5% of urea was added, with stirring, to a viscose containing about 7.8% sodium hydroxide and about 7.5% cellulose, by weight, and having a salt point of 5.1. The viscose was then spun into an aqueous bath containing about 10.6% sulfuric acid, about 3% zinc sulfate and about 18% sodium sulfate to produce a 40 filament, 150 denier yarn which was given a godet stretch of 53%. On testing, the yarn was found to have a dry breaking toughness of 54.4 g. cm./d. cm., and average stiffness of 11.2; wet breaking toughness of 45.7 g. cm./ d. cm., and wet average stiffness of 5.2. This compared with a dry breaking toughness of 48.8 g. cm./d. cm., and average stiffness of 12.6; wet breaking toughness of 34.7 g. cm./d. cm. and Wet average stiifness of 5.7 for a yarn spun from the same viscose, under the same conditions, but in the absence of urea.
Example 4 A yarn was produced from a viscose as described in Example 3, containing 2.5% urea by weight. The spinning conditions were the same as in Example 3 except that the yarn was given a godet stretch of 73%. The yarn had a dry breaking toughness of 51 g. cm./d. cm. and average stiffness of 17.5; wet breaking toughness of 36.1 g. cm./d. cm. and Wet average stifiness of 9.5, as compared to a dry breaking toughness of 37.7 g. cm./ d. cm. and average stiffness of 20.6, and wet breakin toughness of 24.2 g. cm./d. cm. and wet average stiffness of 11.5, for a yarn produced under the same conditions, from a viscose of the same cellulose and sodium hydroxide content, but not containing urea.
7.3% cellulose, and having a salt point of 5.4. The viscose having the urea admixed with it was then spun into an aqueous bath containing about 11.1% sulfuric acid, about 4.8% zinc sulfate, and about 19.8% sodium sulfate, to produce a 40 filament, denier yarn which was given a stretch of about 44% between godets. This yarn had a dry breaking toughnes of 48.1 g. cm./d. cm. and average stiffness of 10.4; wet breaking toughness of 40.3 g. cm./d. cm. and wet average stiffness of 4.9. A similar yarn, from a viscose of the same sodium hydroxide and cellulose content, and of the same salt point, obtained under the same conditions, but in the absence of urea admixed with the viscose, had a dry breaking toughness of only 45 g. cm./d. cm. and average stiffness of 13.5; wet breaking toughness of 33.6 g. cm./d. cm. and wet average stiffness of 5.9.
Example 6 5% of urea was added with stirring to a vis cose containing about 7.5% sodium hydroxide: and about 7.6% cellulose, and having a salt point of 5.4. The viscose was then spun into an aque-- ous bath containing about 10.9% sulfuric acid, about 4.7% zinc sulfate, and about 20% sodium. sulfate, to produce a 40 filament, 150 denier yam which was given a godet stretch of about 65%.. The yarn was then after-treated and dried in the usual way. The dried yarn had a dry breaking: toughness of 51.4 g. cm./d. cm. and average stiffness of only 14.9; wet breaking toughness of 32.2; g. cm./d. cm. and wet average stiffness of 4.9.. Yarn obtained from a viscose of the same fundamental composition but which did not contain'. urea was found to have a dry breaking tough-- ness of only 44.4 g. cm. /d. cm. and average stiffness as high as 18.8; wet breaking toughness of" 25.5 g. cm./d. cm. and wet average stiffness. of 9.8.
As is apparent from the foregoing examples;
the fibers and yarn spun in accordance with the. conventional wet spinning technique from a viscose containing the indicated small amounts of urea are distinguished by increased breaking? toughness and decreased average stiffness by vir-- tue of which they are especially well adapted; to use in which they are subjected to severe: stresses and strains, such as the flexing to which: yarns comprising tire cords are exposed. The fibers and yarns have generally increased tensile: strengths ranging from about 2.7 to 3 gms/denier and high elongations of from about 17 to 23%.
As has been indicated, the salt point of the viscose may be from 3 to 6, and the amount of. urea present may be from 1 to 5%. Generallyspeaking, the influence of the urea on the breaking toughness and average stiffness of the yarns:v and fibers obtained from any given viscose con-' taining normal amounts of cellulose and sodium. hydroxide, within the ranges indicated, is most?- pronounced, the lower the salt point of the viscose. within the stated range of 3 to 6. At salt points; of from say, 3 to 4, the effects of the urea on. the breaking toughness and average stiffness are: more pronounced even when the urea is present; in the smaller amounts.
The urea exerts its modifying effects on the properties of the fibers either prior to or duringtheir spinning or at any rate prior to final setting up of the fibers. The fibers, after their with-- drawal from the bath and after-processing in; accordance with the usual procedures, including: final washing, are found to be substantially en-- tirely free of urea.
Since it will be obvious that changes and varia-- tions maybe made incarrying out the invention,.
t hi 5 it will be understood that the invention is not to be limited except as defined in the appended claims.
I claim:
1. A fiber-forming composition consisting of a mixture of viscose containing, by weight, from about 6 to about 8% of sodium hydroxide and from about 6 to about 8% of cellulose, and havin a sodium chloride salt test value of from 3 to 6, with from 1 to 5% by weight of urea.
2. As a fiber-forming composition, a mixture of viscose with about 1 to 5% by weight of organic water-soluble material consisting of urea, the urea being the sole organic water-soluble material in the mixture, said composition having normal ageing characteristics.
3. As a fiber-forming composition, a mixture of viscose containing about 6 to about 8% of sodium hydroxide by weight and about 6 to about 8% by weight of cellulose, with about 1 to 5% by weight of organic water-soluble material consisting of urea, the urea being the sole organic water-soluble material in the mixture, the composition having -a. sodium chloride salt point oil 3 to 6.
GEORGE ALVIN RICHTER, JR.
References Cited in the file of this patent