US3108849A - Process for producing viscose regenerated cellulose fibers - Google Patents

Process for producing viscose regenerated cellulose fibers Download PDF

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US3108849A
US3108849A US147507A US14750761A US3108849A US 3108849 A US3108849 A US 3108849A US 147507 A US147507 A US 147507A US 14750761 A US14750761 A US 14750761A US 3108849 A US3108849 A US 3108849A
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cellulose
viscose
coagulating bath
concentration
sulfuric acid
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US147507A
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Owashi Toshiro
Onoe Keigo
Ito Hiroshi
Kawai Atsushi
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Mitsubishi Chemical Corp
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Mitsubishi 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
    • D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
    • 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

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  • the present invention relates to an improved process for preparing viscose regenerated cellulose liber having properties of a high Youngs -modulus in wet state, a low Water swelling, a high strength, and a high knot strength and a good dyeability and having a tineness of 0.5-30 denier, and to an improved process for preparing such denier.
  • the ber thus obtained in spite of having a low water swelling, a high strength, and a high fatigue resistance, posses a low Youngs modulus in Wet state, so that the fabric obtained therefrom is inadequate for a practical usage because of a large shrinkage after washing and a bad dimensional stability. It has also been proposed that a highly viscous viscose solution be subjected to a spinning process in an unripened state as indicated in the U.S. Patent No. 2,732,- 279.
  • the fiber prepared by the said lmethod possesses a low water swelling and a high Youngs modulus in wet state, while it has an extremely lower knot strength and a lower fatigue resistance, so that the fabric prepared therefrom has a poor abrasion resistance.
  • fiber having a high Youngs modulus in Wet state may be prepared by extruding a viscose solution into a coagulating bath which contains sulfuric acid, sodium sulfate and Zinc sulfate as described in the Belgian Patents No. 573,565 and No. 581,- 631.
  • the bers obtained by these methods have inferior properties such as strength, knot strength, fatigue resistance and dyeability.
  • the object of the present invention is to provide an improved process for manufacturing viscose regenerated cellulose fiber having a high Youngs modulus in -Wet state, a low Water swelling, a high strength, a high knot strength and a good dyeability,
  • A represents an alkali concentration (percent) in the viscose solution
  • B is a sodium sulfate concentration (percent) in a coagulating bath
  • C is a zinc sulfate concentration (percent) in a coagulatin-g bath
  • D stands for a single filament denier of the ber to be spun.
  • the viscose regenerated cellulose liber prepared by the -method'shown in FIG. 6, a flow sheet of the process has a higher Youngs modulus in wet state, a lower Water swelling, a higher strength, especially in Wet state, andv a higher knot strength as compared with those of viscose fibers obtained by a conventional method. Consequently, the fabric converted-from the ber prepared by the method of this invention has characteristics of an extremely small shrinkage after Washing, an extremely high dimensional stabiility, a high tear strength, a high abrasion resistance, and a good dyeability, and what is more, when the textile is subjected to a resin treatment, thus treated textile has also a good crease resistance, and a good abr-asion resistance.
  • the pulp is steeped into an aqueous caustic soda solution, pressed to remove the excess amount of aqueous caustic soda solution therefrom and shredded.
  • the shredded alkali cellulose is xanthated after ageing; however, the alkali cellulose may be xanthated immediately after shredding.
  • alkali cellulose For the purpose of xanthation of alkali cellulose, it may be preferable to employ 40% to 50%, based upon the weight of cellulose in the alkali cellulose, of carbon disulde.
  • the produced sodium cellulose xanthate is added with Iwater and aqueous caustic soda solution and dissolved therein to make a viscose solution.
  • the degree of polymerization of cellulose in the viscose solution is preferred to be in the range from 350 to 700, and especially ⁇ from 400 to 500.
  • the viscosity of the viscose solution is an important factor of the present invention, and it must be a value Within a range from to 500 poises at spinning.
  • viscosity of viscose solution When the viscosity of viscose solution is less than 100 poises, the solution can not effectively be spun, and when more than 500 poises, it may also be difficult to spin and thus the obtained ber has a deteriorated quality.
  • the most preferable viscosity is -400 poises.
  • the cellulose concentration of viscose may advantageously be determined in accordance with the degree of polymerization of the cellulose. For example, when the degree of polymerization of cellulose is 430, it is preferable to employ about 7% of the cellulose concentration.
  • the alkali concentration in the viscose solution is settled within a range from 3% to 5%. When the alkali concentration is out of these limits, it results in a decrease in spinnability of the solution.
  • the obtained viscose is subsequently iiiltered, deae-rated, ripened and extruded into a coagulating bath.
  • the degree of ripening of the viscose at the time of spinning is also one of the important factors of the present invention.
  • the salt point of the viscose solution at spinning time is within the limits of between 9 and 20.
  • the liber prepared from the viscose having a salt point less than 9 has a lower strength and a higher water swelling.
  • an excessively high salt point of more than 20 results in the spinning conditions becoming worse.
  • the most preferable salt point is between 12-16.
  • a bath containing zinc sulfate, sodium sulfate and sulfuric acid may be employed.
  • the zinc sulfate concentration of the coagulating bath is one of the most important factors of the present invention, and it must be within the limits of from 0.02% to 0.04%.
  • the zinc sulfate concentration is less than 0.02%, the fiber thus obtained will have inferior characteristics such as knot strength and dye absorption, while in case of more than 0.04%, it will deteriorate the properties such as strength in wet state, knot strength and dye absorption.
  • the curve 1 shown in FIG. 1-FIG. 3 represents the correlation between the zinc sulfate concentration in a coagulating bath and the quality of fiber obtained by the method which comprises extruding a viscose solution containing 7% of cellulose and 4% of alkali and having a viscosity of 170 poises and salt point of 16, into a coagulating bath containing 1.5% of sodium sulfate, 1.33% of sulfuric acid and various concentrations of zinc sulfate, the temperature of which is kept at C. and the immersion length of which is 40 cm., through a spinneret (0.06 hole diameter and 1000 holes), subjecting the freshly spun thread to 80% stretch within air, taking the thread on a reel at a spinning velocity of 18 m./ min. and then subjecting to refining in accordance with a conventional method. From the said curves, a specific effect of zinc sulfate employed in the present invention can clearly be understood.
  • the concentration of sodium sulfate may practically be within the limits of between 1% and 10%, and preferably be from 1% to 5%. When the concentration of sodium sulfate becomes more than 10%, it is difficult to spin the viscose solution. An employment-of less than 1% is not practicable from an economical point of view.
  • the concentration of sulfuric acid has a close correla tion with the lalkali concentration of viscose solution, sodium sulfate concentration and zinc sulfate concentration of coagulating bath, and with single filament denier of the ber to be spun. lt must. be within the limits provided by the following equations:
  • the minimum sulfuric acid concentration (percent) wherein A represents the concentration (percent) of alkali in a viscose solution, B is the concentration (percent) of sodium sulfate in a coagulating bath, C is the concentration (percent) of zinc sulfate in a coagulating bath, and D stands for the single lilament denier (d.) of the ber to be spun.
  • concentration of sulfuric acid is below the above defined limits, it is vdiiiicult to spin the viscose solution, and on the other hand, when the concentration is above these limits, it is observed that the spinnability of the solution delinitely decreases.
  • the specific effect of zinc sulfate is not known, but the obtained liber has a lower knot strength and a lower dye absorption.
  • the curve 2 shown in FIG. l-FIG. 3 represents the correlation of between the zinc sulfate concentration and the quality of fiber prepared by using the same conditions with those of curve l except that the concentration of sulfuric acid is 2.3%.
  • the minimum sulfuric acid concentration in a coagulating bath of the present invention becomes higher and higher in accordance with the increases in the concentration of alkali in the viscose solution, in the concentration of sodium sulfate in a coagulating bath and in the single filament denier of the fiber to be spun, while it becomes lower and lower in accordance with the increase in the zinc sulfate concentration.
  • the maximum sulfuric acid concentration it becomes higher and higher in accordance with the increases in the alkali concentration in the viscose solution, in the sodium sulfate concentration and the zinc sulfate concentration in a coagulating bath, and also in the single filament denier of the fiber to be spun.
  • a temperature of between 10 and 30 C. may practicably be employed, and its preferable range is from 15 to 25 C.
  • a temperature of more than 30 C. is employed, it must result a diiiicult problem of spinning.
  • a stabilizing tube is provided near the spinncret to make the coagulating bath liquid flow in the same direction as the liber therethrough. This method is especially effective in the case when a spinneret having less than holes is employed.
  • a preferable immersion length of the coagulating bath is 20-50 cm. When the immersion length is out of this range, it results in decreased spinnability.
  • the thread brought out from the coagulating bath is stretched in the air or in a second bath.
  • the fiber stretched inthe second bath has a higher tensile strength and higher knot strength than that stretched in the air. However, it is preferable to stretch the liber in -a second bath.
  • stretched liber is then subjected to a refining process according to a conventional method.
  • Example 1 A wood pulp, the polymerization degree of which was 800, was steeped into 19% :aqueous caustic soda solution containing 0.85% of hemicellulose at 22 C. for 50 minutes, and then pressed to 2.75 times the dried pulp. Thus obtained alkali cellulose was shredded at 25 C. for 1 hour, and aged for 15 hours at 24 C. to give an alkali cellulose having 500 of polymerization degree. To this 47%, based upon the weight of cellulose in the alkali cellulose, of carbon disulfide was added. The alkali cellulose was then subjected to Xanthation at 26 C.
  • N ern-Wet modulus oi ber means force (gld.) required to elongate the fiber by 5% in Wet state.
  • Example 1 For the purpose of reference, the same procedures as in the Example 1 were repeated except that ythe following baths were employed respectively instead of the previously described coagulating bath.
  • Example 2 tained fiber was shown as following.
  • the polymerization degree of cellulose in the viscose solution was 400.
  • the viscose solution was iltered, deaerated, and then ripened at 3 C. for a short while.
  • the viscose solution having poises of viscosity and a salt point of 16
  • Example 4 A Wood pulp, the polymerization of which w 800, was steeped into 19% aqueous caustic soda solution at 22 C. for 50 minutes, pressed to 2.75 times the dried pulp, shredded at 26 C. for 1 hour, and aged at 26 C. for 8 hours to give an alkali cellulose. To the alkali cellulose, 47%, based upon the Weight of cellulose in the said alkali cellulose, of carbon disulfide was added. The alkali cellulose was subjected to Xanthation at 26 C. for 140 minutes. The obtained sodium cellulose Xanthate was diluted with aqueous caustic soda solution and water to give a viscose solution having 7.3% of cellulose and 4.5% ⁇ of alkali.
  • the polymerization degree of cellulose in the viscose was 500.
  • the viscose solution was ltered, deaerated and then ripened.
  • the obtained viscose solution having 400 poises of viscosity and a salt point of 16 was extruded through a spinneret (0.07 mm. hole diameter and 1000 holes) into a coagulating bath containing 0.02% of zinc sulfate, 1.0% of sodium sulfate and 1.35% of sulfuric acid and being kept at 18 C.
  • the immersion length of the coagulating bath was 30 cm.
  • the thread brought out from the coagulating bath was subjected to 105% stretch in the second bath containing 4% of sulfuric acid and being kept at 50 C., and then to a rening process.
  • the quality of thus obtained fiber was shown as follows:
  • a Wood pulp the polymerization degree of which was 800, was steeped into 19% aqueous caustic soda solution at 20 C. for 50 minutes, pressed to 2.75 times the dried pulp, shredded at 26 C. for 1 hour, and then aged at 26 C. for 8 hours.
  • To the obtained alkali cellulose 50%, based upon the weight of cellulose in the alkali cellulose, of carbon disulfide was added.
  • the alkali cellulose was subjected to a Xanthation at 26 C. for 150 minutes to give sodium cellulose Xanthate.
  • the sodium cellulose Xanthate was diluted with aqueous caustic soda solution and water to give a viscose solution containing 6% of cellulose and 3.0% of alkali.
  • the polymerization degree of cellulose in the viscose was 500. It was filtered, deaerated and r-ipened. Thus obtained viscose solution having 200 poises of viscosity and a salt point of 16 was extruded through a spinneret (0.08 mm. hole diameter and 1000 holes) into a coagulating oath containing 0.03% of zine sulfate, 1.5% of sodium sulfate and Tensile strength (sid.)
  • the sodium cellulose Xanthate was diluted with aqueous caustic soda solution and water to give a viscose solution containing 4.5% of cellulose and 4.5% of alkali.
  • the polymerization degree oi cellulose yin the viscose was 600.
  • the Viscose solution was filtered, deaerated an dripened.
  • ⁇ Thus obtained viscose solution having poises of viscosity and a salt point of l5 was extruded through a spinneret (0.04 mm. hole diameter and 1000 holes) into a coagulating bath contain ing 0.02% of Zinc sulfate, 1.5% of sodium sulfate and 1.4% of sulfuric acid and being kept at 18 C.
  • the immersion length of the coagulating bath was 20 cm.
  • the thread brought out from the coagulating bath was subjected to 98% stretch in the second bath containing 2% of sulfuric acid at 80 C. and then subjected to refining.
  • the quality of thus obtained liber was shown as follows:
  • alkali cellulose was added with 43%, based iupon the Weight of cellulose in the alkali cellulose, of carbon disuliide.
  • the alkali cellulose solution was xanthated at 27 C. for 150 minutes to give sodium cellulose xanthate.
  • the sodium cellulose Xanthate was diluted by adding aqueous caustic soda solution and Water to give a ,viscose solution containing 9% of cellulose and 5% of alkali.
  • the polymerization degree of celluose in the viscose was 400.
  • the viscose solution was iiltened, deaerated and ripened.
  • This fiber had a circular cross section.
  • Example 8 A wood pulp, the polymerization of which was 800, was steeped as -a slurry into 17.5% aqueous caustic sod-a solution at 45 C., ypressed to 2.8 times the dried pulp, shredded and aged in a room kept at 27 C. for 4 hours.
  • alkali cellulose To the obtained alkali cellulose, 60%, based upon the weight of cellulose in the alkali cellulose, of carbon disulde was added, and the alkali cellulose solution was subjected to xanthation at 26 C. for 140 minutes to give a sodium cellulose xanthate.
  • the sodium cellulose xanthate was diluted with aqueous caustic soda solution and Water to give a viscose solution containing 7% of celluose and 4% of alkali.
  • the polymerization degree of cellulose in the viscose was 380.
  • the viscose solution was then iltered, deaerated and ripened.
  • the obtained viscose having 100 poises of viscosity and a salt point of 20 was extruded through a spirineret (0.07 mm. hole diameter and 50 holes) into a coagulating bath containing 0.03% of zinc sulfate, 2% of sodium sulfate and 1.3% of sulfuric -acid and being kept at 20 C.
  • a glass stabilizing tube of 8 mm. inner diameter and 40 cm. length was settled at the position 1 cm.off from the spinneret. :T he coagulating bath liquid was made llow with the thread and in the same direction as the thread Within the glass tube.
  • the flow velocity of the coagulation solution in the glass tube was 18 m./min., and the peripheral speed ofthe iirst roller was 20 rn./ min.
  • the gel liber passed through the glass tube was subjected to 170% stretch within air.
  • Example 9 aqueous caustic soda and water to give a viscose solutioncontaining 7% of cellulose yand 4% of alkali.
  • the polymerization degree of cellulose in the viscose solution was 430.
  • the viscose solution was then iiltered, deaerated and aged.
  • the ripened viscose solution having 208 poises of viscosity and a salt point of 18 was extruded through a spinneret (0.06 mm. hole diameter and 1000 holes) into a coagulating bath containing 0.04% of zinc sulfate, 10% of sodium sulfate and 1.7% of sulfuric acid and being kept at 20 C.'
  • the irrnnersion length of the coagulating bath was 40 cm.
  • the thread brought :out from the coagulating bath was subjected to 110% stretch in the second bath containing 2% of sulfuric acid and being kept at 80 C., and then subjected to a refining process.
  • Example 11 The same vislcose solution as shown in Example 1 was extruded through a spinneret (0.09 min. hole diameter and 1500 holes) into a coagulating bath containing 0.03% of zinc sulfate, 1.5% of sodium sulfate and 1.9% of sulfuric acid and being kept at 20 C.
  • the thread brought out from the coagulating bath was subjected to 70% stretch Within air and then to a rening process.
  • the obtained liber had the following properties:
  • Example 12 The same viscose solution as shown in Example l was extruded through a Spinnerei (0.10 mm. hole diameter and 1000 holes) into a coagulating bath containing 0.03% of zinc sulfate, 1.5% of sodium sulfate and 2.6% of sulfuric acid and being kept at 20 C. The thread brought out from the coagulating bath was subjected to 65% stretch within air, and then subjected to reiining.
  • the ber had a circular cross section.
  • Example 13 The same viscose solution as shown in Example 2- was extruded through a spinneret (0.08 mm. hole diameter and 6000 holes) into a coagulating bath containing 0.03% of zinc sulfate, 1.6% of sodium sulfate and 1.65% of sulfuric acid and being kept at C. The immersion length of the bath was 45 cm. The extruding rate of the viscose was 320 cc./min. The thread removed from the coagulating bath was subjected to 45% stretch within air, to a regeneration process in the second bath containing 2% of sulfuric acid and being kept at 80 C., and then subject to refining. The spinning velocity was 14 m./ min. Thus obtained fiber had the following properties.
  • Example 14 The same viscose solution as shown in Example 2 was extruded .through a spinneret (0.12 mm. hole diameter and 700 holes) into a coagulating bath, the immersion length of which was 45 cm. and the temperature of which was kept'at 20 C., containing 0.03% of zinc sulfate, 3.2% of sodium sulfate and 2.1% of sulfuric acid.
  • the extruding rate of the viscose solution was 300 cc./min.
  • the thread removed from the coagulating bath was subjected to 35% stretch in the air, and treated in a regeneration process in the second bath containing 2% of sulfuric acid maintained at 80 C., and then subjected to refining.
  • the spinning velocity was 22 m./min.
  • Thus obtained fiber had the following properties.
  • the ber obtained in the present example had a circular cross section.
  • said viscose solution has a cellulose polymerization degree of from 400 to 500, a viscosity of from to 400 poises and a salt point of from 12 to 16 is extruded into a coagulating bath containing from 1 to 5% of sodium sulfate and having an immersion length of from 20 to 50' cm.
  • a method according to claim 1 which comprises xanthating an alkali cellulose with the addition of carbon disulfide in an amount 40 to 50% by weight on the basis of the cellulose in said alkali cellulose, dissolving the xanthated alkali cellulose in an aqueous caustic solution to form a Viscose solution containing from 3 to 5% of alkali having a cellulose polymerization degree of from 400 to 500, a viscosity of from 150 to 400 poises, and a salt point of from 12 to 16, extruding the solution into a coagulating bath containing from 0.02 to 0.04% of zinc sulfate, from 1 to 5% of sodium sulfate and sulfuric acid at a concentration Within the range defined by the equa ⁇ tions minimum sulfuric acid concentration (percent)l wherein A represents the alkali concentration (percent) in the viscose solution, B is the sodium sulfate concentration (percent) in the coagulating bath, C is the zinc s

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US147507A 1960-10-27 1961-10-25 Process for producing viscose regenerated cellulose fibers Expired - Lifetime US3108849A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3324216A (en) * 1962-05-16 1967-06-06 Toyo Spinning Co Ltd Viscose spinning process
US3341645A (en) * 1963-03-07 1967-09-12 Teijin Ltd Method of producing viscose rayon staple and a spinning apparatus for use in the method
US3352957A (en) * 1962-11-06 1967-11-14 Chimiotex Process for spinning cellulosic fibers
US3381075A (en) * 1962-05-28 1968-04-30 Teijin Ltd Process for preparation of viscose regenerated cellulose fibers
US3419652A (en) * 1963-09-10 1968-12-31 Mitsubishi Rayon Co Process for producing highly crimped fibers
US3506754A (en) * 1967-09-27 1970-04-14 Tachikawa Res Inst Process for manufacturing rayon having high degree of polymerization by the viscose process
CN116876092A (zh) * 2023-07-11 2023-10-13 河北铭威工程设计有限公司 一种特高湿模量变化型莫代尔纤维及其制备工艺

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013002833B4 (de) 2013-02-19 2017-03-23 Deutsche Institute Für Textil- Und Faserforschung Denkendorf Verfahren zur Herstellung von Celluloseregeneratfasern und Verwendung der nach dem Verfahren hergestellten Celluloseregeneratfasern

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2997365A (en) * 1958-08-12 1961-08-22 Courtaulds Ltd Production of regenerated cellulose filaments

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2997365A (en) * 1958-08-12 1961-08-22 Courtaulds Ltd Production of regenerated cellulose filaments

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3324216A (en) * 1962-05-16 1967-06-06 Toyo Spinning Co Ltd Viscose spinning process
US3381075A (en) * 1962-05-28 1968-04-30 Teijin Ltd Process for preparation of viscose regenerated cellulose fibers
US3352957A (en) * 1962-11-06 1967-11-14 Chimiotex Process for spinning cellulosic fibers
US3341645A (en) * 1963-03-07 1967-09-12 Teijin Ltd Method of producing viscose rayon staple and a spinning apparatus for use in the method
US3419652A (en) * 1963-09-10 1968-12-31 Mitsubishi Rayon Co Process for producing highly crimped fibers
US3506754A (en) * 1967-09-27 1970-04-14 Tachikawa Res Inst Process for manufacturing rayon having high degree of polymerization by the viscose process
CN116876092A (zh) * 2023-07-11 2023-10-13 河北铭威工程设计有限公司 一种特高湿模量变化型莫代尔纤维及其制备工艺

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DE1469108A1 (de) 1968-12-05
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