US3107970A - Process for the manufacture of high tenacity viscose rayon - Google Patents

Process for the manufacture of high tenacity viscose rayon Download PDF

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Publication number
US3107970A
US3107970A US141356A US14135661A US3107970A US 3107970 A US3107970 A US 3107970A US 141356 A US141356 A US 141356A US 14135661 A US14135661 A US 14135661A US 3107970 A US3107970 A US 3107970A
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Prior art keywords
viscose
bath
spinning
liter
temperature
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US141356A
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English (en)
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Kusunose Masatomo
Saji Yasuo
Koyasu Takeo
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Teijin Ltd
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Toho Rayon Co Ltd
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08—Composition of the spinning solution or the bath
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S264/00—Plastic and nonmetallic article shaping or treating: processes
    • Y10S264/27—Process of spinning viscose where viscose has high degree of polymerization

Definitions

  • PROCESS FOR THE MANUFACTURE OF HIGH TENACITY VISCOSE RAYON Filed Sept. 28, 1961 United States Patent 3,107,970 PROCESS FOR THE MANUFACTURE OF HIGH TENACITY VISCOSE RAYON Masatomo Kusunose, Yasuo Saji, and Takeo Koyasu, all of Itano-gun, Tokushima, Japan, assign'ors to Toho Rayon Kabushiki Kaisha, Tokyo, Japan, a corporation of Japan Filed Sept. 28, 1961, Ser. No. 141,356 Claims priority, application Japan Oct. 4, 1960 4 Claims. (Cl.
  • the present invention rel-ates to a process for the manufacture of viscose rayon, which comprises heating unaged viscose to a temperature above that of la spinning bath, extruding the thus heated viscose in a low temperature acidic sulfate bath containing formaldehyde, and stretching the resulting threads in a second bath, namely in a double bath stretching method.
  • a type of viscose sufficiently removed of so-called structure is shaped to filaments by an extremely slow regeneration and then by imparting resulting filaments crystallization and arrangement eifects substantially simultaneously to impart the regenerated fiber a highly crystalline property and orienta tion.
  • the substance of the present invention is based on a knowledge that an excellent fiber of a high wet tensile strength can be obtained by heating a relatively insuificiently aged viscose at high temperatures to decompose so-ca-lled structure for improving dispersion property and regenerating by introducing thus treated viscose into a spinning bath which contains formaldehyde and is kept at a temperature lower than that of the viscose at least by 20 C.
  • the quantity of carbon bisulfide required for the manufacture of viscose in the practice of this invention ranges from 35 to 55% of the amount of cellulose used and, in addition, no particularly high 'y-value is required.
  • the required alkali content of the viscose is in a range of 0.5 to 0.9 times its content of cellulose, and a departure from such a range results in degradation of the product obtained.
  • High viscosity viscose which viscosity varies from 50 to 400 seconds and preferably higher than 100 seconds, should be used. From viscose of a viscosity below 50 seconds a fragile product of a poor knot strength can only 'be obtained. 1 According to the present invention, viscose is used after it has been heated from 45 to C. and a range from 55 to 66 C. is optimum. Various apparatus and methods are used for'hea-ting viscose. It is necessary to heat the viscose rapidly and uniformly as much as possible near the spinneret.
  • viscose is heated by providing a heat exchanger whose heat source is heated water in the neighborhood of the spinneret.
  • Such heated viscose should be spun in a spinning bath of a temperature held at least 20 C. below that of the viscose.
  • the thus heated viscose is kept from being cooled by the low temperature of the spinning bath at a part of the viscose pipe immediately before the spinneret immersed in the spinning bath.
  • the spinning bath according to this invention is 35 C. maximum bath containing from 50 to 150 gin/liter Na SO from 1. to 10 gm./ liter formaldehyde, 30 gm./liter. max. ZnSO; and 40 gin/liter min. H
  • the spinning operation lacks smoothness to lower the quality of products.
  • concentration of Na SO is less than 50 gm./ liter, variation in concentration due to Na SO which occurs in the spinning bath is high and the process control and preparation of the spinning bath become difficult.
  • the essential requirement for the present invention is heating viscose in such a way that the temperature of the viscose entering the spinning bath may be at least 20 C. higher than that of the spinning bath and moreover above 40 C.
  • the viscose is spun in an ordinary process, a remarkably inferior quality product can only be obtained as compared with the case with the present invention.
  • the present invention is carried out according to the double bath stretching spinning process and if necessary a third or a higher number of baths may be used.
  • the most remarkable feature of the regenerated cellulose fiber obtained in this invention is a high wet modulus. This is numerically compared by tension (grnz) per denier required for 5% elongation on the load-elongation curve (FIGURE 1) when wet.
  • the present inventor h z s made various experiments on the effect of the rates of stretching or elongations (percent) X, Y and Z upon the strength of the threads obtained. If the velocity of filaments being reeled on the first spool from the first bath is a m./'min.; that of the filaments being reeled on the second spool after passing through the second 'bath (i.e. the first stretching bath) is b m./min.; and that of the filaments being reeled on the third spool after passing through the third bath (i.e. the second stretching bath) is c m./min., the elongation X (percent) in the first stretching bathis:
  • Hot weak acidic water baths are used at above C. for the second and third baths; in the second bath, tion within which no local breakage of threads occurs is 180%. In thls case,stretching could not beefiected in the third bath and the reeling was carried out around the final spool at the velocity of 35 nth/mm. after passing same through the third bath.
  • Both the second and third baths were used at 90 0.; stretching was given in the second bath and the maximum tolerance of 15% stretching was given in the third bath.
  • the above-mentioned fibers (a) and (b) were immersed in 5% aqueous NaOH solution at 20 C. for 10 minutes a without tension, thoroughly washed in dilute acetic acid and water and dried and then their strength was determined and the result was shown as percentages to the corresponding strength of the original sample as in'Ilable 3.
  • the fibersaccording to this invention show evidently the maximum tolerance of elonga-- small lowering of strengths due to above mentioned alkali treatment.
  • Example 1 Alkali which was prepared according to the ordinary way by steeping, pressing, and shredding from wood pulp, was aged for a short interval of time, then xanthated and dissolved in 50% by weight of cellulose of carbon bisulfide to produce viscose comprising 7% cellulose and 4.5 alkali content. Such viscose was then filtered and defoamed, when the temperature was kept as low as possible during the Whole treatment from xanthation to spinning, and the viscose of 218 second viscosity and 15 salt index was spun into a spinning solution comprising 100 gm./liter Na SO 65 gm./liter H SO and 5 gun/liter formaldehyde at 30 C.
  • Such spun filaments were stretched to 230% in a slightly acidic second bath at 90 C., reeled, cut and purified in an ordinary process.
  • the qualities of products thus obtained are shown under (e) of the following table.
  • Alkali cellulose which was obtained by steeping and shedding from wood pulp in an ordinary process, was aged for a short interval of time and xanthated by using 38% carbon bisulfide of the weight of cellulose, then viscose was prepared to 8% cellulose and 5% alkali.
  • Such viscose was filtered and deaerated, with the operational temperature being held as low as possible from dissolving to spinning.
  • Wood pulp was steeped, squeezed and shredded to ob- 'tain alkali cellulose.
  • the resulting cellulose was aged in a short interval of time and xanthated using 40% carbon bisulfide based on the weight of cellulose used and further added 10% carbon bisulfide based on the weight of cellulose used at the beginning of xanthation.
  • Such viscose contained 7% cellulose and 4.5% alkali, which was filtered and deaerated.
  • the viscose was spun at viscosity 108 second and salt index of 18.2.
  • the spinning was performed at the operational temperature held as low as possible in a treatment from xanthation to spinning and in the spinning bath containing 65 gm./liter H SO '95 gin/liter N-a SO and 6 gm./ liter formaldehyde at 28 0., through a 4000 hole spinneret of 0.06 diameter.
  • Said viscose was heated immediately before spinning to 56 C. by passing through a heat exchanger secured between a gear pump and curved spinning pipe, of which heat source was hot water.
  • Spun filaments were passed through a second 2-meter bath containing 30 gin/liter H S0 and 50 gn1./liter Na SO at 30 C., While stretching was given to the filaments. Further, said filaments Were passed through a third bath of 1.5 meters, containing 60 gm./ liter H 80 and 100 gm./liter Na SO at 90 C., while the filaments were imparted 50% stretching.
  • the total stretching in the second and third baths are 245
  • the filaments were reeled around the final spool at a velocity of 35 art/min. and cut and purified by usual process.
  • the properties of the filaments were as shown in Table 2.
  • a process for manufacturing high tenacity viscose rayon filaments comprising heating to a temperature in the range of between 45 C. and 70 C. an unripened viscose having a salt index above 9 and having a viscosity ranging from 50 to 400 seconds, said viscose having an alkali content ranging from 0.5 to 0.9 times the cellulose content, then spinning said viscose in its heated state into an acid coagulating bath held at a temperature in the range of between a maximum of 35 C. and a minimum of below the viscose temperature by at least 20 C., said acid coagulating bath containing from 50 to gm./liter Na SO from 1 to 10 gm./liter formaldehyde, 30 gm./liter maximum.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
US141356A 1960-10-04 1961-09-28 Process for the manufacture of high tenacity viscose rayon Expired - Lifetime US3107970A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP4019560 1960-10-04
JP2053961 1961-06-09

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US3107970A true US3107970A (en) 1963-10-22

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US (1) US3107970A (no)
BE (1) BE608811A (no)
DE (1) DE1261978B (no)
FI (1) FI40920B (no)
GB (1) GB993786A (no)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3226461A (en) * 1962-02-27 1965-12-28 Courtaulds North America Inc Manufacture of regenerated cellulose fibers from viscose
US3277226A (en) * 1962-04-09 1966-10-04 Fmc Corp Viscose rayon fiber and method of making same
US3337671A (en) * 1958-07-31 1967-08-22 Chimiotes S A Method of making regenerated cellulose filaments
US3388117A (en) * 1963-03-28 1968-06-11 Courtaulds North America Inc Filaments of regenerated cellulose
US3419652A (en) * 1963-09-10 1968-12-31 Mitsubishi Rayon Co Process for producing highly crimped fibers
US3434913A (en) * 1964-12-28 1969-03-25 Fmc Corp Viscose rayon fiber and method of making same
US3494996A (en) * 1965-07-20 1970-02-10 Itt Rayonier Inc Method for producing high tenacity rayon

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2611928A (en) * 1948-11-23 1952-09-30 American Viscose Corp Method for producing high tenacity artificial yarn and cord
US2705184A (en) * 1949-08-25 1955-03-29 Textile & Chemical Res Company Process for the production of rayon products
US2937070A (en) * 1955-08-02 1960-05-17 Du Pont Viscose process
GB854152A (en) * 1957-06-21 1960-11-16 Glanzstoff Ag Improvements relating to the production of spun threads by viscose spinning

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2611928A (en) * 1948-11-23 1952-09-30 American Viscose Corp Method for producing high tenacity artificial yarn and cord
US2705184A (en) * 1949-08-25 1955-03-29 Textile & Chemical Res Company Process for the production of rayon products
US2937070A (en) * 1955-08-02 1960-05-17 Du Pont Viscose process
GB854152A (en) * 1957-06-21 1960-11-16 Glanzstoff Ag Improvements relating to the production of spun threads by viscose spinning

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3337671A (en) * 1958-07-31 1967-08-22 Chimiotes S A Method of making regenerated cellulose filaments
US3226461A (en) * 1962-02-27 1965-12-28 Courtaulds North America Inc Manufacture of regenerated cellulose fibers from viscose
US3277226A (en) * 1962-04-09 1966-10-04 Fmc Corp Viscose rayon fiber and method of making same
US3388117A (en) * 1963-03-28 1968-06-11 Courtaulds North America Inc Filaments of regenerated cellulose
US3419652A (en) * 1963-09-10 1968-12-31 Mitsubishi Rayon Co Process for producing highly crimped fibers
US3434913A (en) * 1964-12-28 1969-03-25 Fmc Corp Viscose rayon fiber and method of making same
US3494996A (en) * 1965-07-20 1970-02-10 Itt Rayonier Inc Method for producing high tenacity rayon

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FI40920B (no) 1969-03-31
GB993786A (en) 1965-06-02
BE608811A (fr) 1962-02-01
DE1261978B (de) 1968-02-29

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