US3539678A - High speed spinning method of viscose rayon filaments having high wet modulus - Google Patents

High speed spinning method of viscose rayon filaments having high wet modulus Download PDF

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US3539678A
US3539678A US660419A US3539678DA US3539678A US 3539678 A US3539678 A US 3539678A US 660419 A US660419 A US 660419A US 3539678D A US3539678D A US 3539678DA US 3539678 A US3539678 A US 3539678A
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viscose
spinning
percent
polymerization
filaments
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US660419A
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Yoichi Uchida
Keniti Hukuma
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Teijin Ltd
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Teijin 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

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  • This invention relates to a high speed spinning method of viscose rayon filaments having high wet modulus, and its object resides in spinning with a horizontal type spinning machine at a spinning speed of at least 80 meters per minute, viscose rayon filaments having high wet modulus as well as excellent touch and good luster.
  • FIG. 1 illustrates one instance of the relationship between the rate of solvent removal of the filaments on the first godet and the fiber properties
  • FIGS. 2a and 2b illustrate the zones of the average degree of polymerization, cellulose content and total alkali content of the viscose used in this invention.
  • FIG. 3 illustrates one instance of the relationship between the heating temperature immediately prior to spinning, the rate of solvent removal on the first godet, spinnability and stretchability.
  • the main point of the technical improvement in the method of spinning viscose rayon concerned the control of the state of coagulation and regeneration of the viscose.
  • Viscose consists of cellulose xanthate dissolved in an alkali solution, and the fiber-forming process is a solvent removal diffusion with reaction from cellulose xanthate to cellulose.
  • rate of solvent removal denotes the rate at which the solvent (the aqueous solution of alkali) is driven out of the viscose and is a ratio of the amount of the solvent removed during the spinning step to the amount of the solvent of the original viscose, expressed as a weight percentage.
  • the cellulose content of the viscose, C is determined in customary manner, while the cellulose content during the spinning step, C is determined in the following manner.
  • About 2 grams of gel filament collected during the step in which the measurement is to be made are dipped in an ice-cooled decomposition stopping solution for about 30 minutes, then subjected to centrifuging for minutes to eliminate the excess liquid and thereafter accurately weighed to obtain the gel weight (A gram).
  • this specimen is dipped for 10 minutes in an aqueous sulfuric acid solution of a concentration 100 g./l. to carry out the regeneration completely. This is followed by washing with water, drying for 3 hours at 100-105 C. and thereafter accurately weighing the product to obtain the weight (B gram). C is then calculated by means of the Equation 4.
  • the first condition concerns the composition of the viscose.
  • DP average degree of polymerization
  • CC cellulose content
  • total alkali content of the viscose we conducted numerous experiments concerning the three factors of the average degree of polymerization (DP) of the viscose and the cellulose content (CC) and total alkali content of the viscose, with the consequence that it was found that the hoped-for end could be achieved when the average degree of polymerization ranged between 400 and 700 and the mutual relationships of these three factors were such that they would fall within the zone indicated by means of the oblique lines in FIGS. 2-a and 2-b. If this zone is represented by mathematical expressions, the previously presented Formulae l and 2, which correspond to FIGS. 2-12 and 2-1), respectively, are obtained.
  • the cellulose and alkali contents of the viscose must be chosen to come within their proper ranges in accordance with the average degree of polymerization of the viscose.
  • the second condition concerns the ripening of the viscose. It was found that the gamma value of the viscose at the time of its spinning must be in the range of 80.
  • the third condition of this invention is the requirement that the viscose be heated at 35-60 C. immediately prior to spinning of the viscose.
  • the viscosity is relatively high owing to the high degree of polymerization of the viscose, and along with the rise in the spinning speed, the viscose viscosity at the time of the extrusion has a very great effect on the state of spinnmg.
  • FIG. 3 One instance of an experiment conducted to show specifically the relationship between the heating temperature, spinnability, stretchability and rate of solvent removal is graphically shown in FIG. 3.
  • the curve (0) drawn with the dotted line represents the spinnability (percent)
  • the curve (d) drawn with the solid line represents the stretchability
  • the curve (e) drawn with the dot-and-dash line indicates the rate of solvent removal.
  • the viscose having a average degree of polymerization of 530, a cellulose content of 5.0%, a total alkali content 4.4% and a gamma value of 73 at the time of spinning, extruded from a spinneret having 75 holes, each 0.06 mm. in diameter, into a 50 C. spinning bath composed of 5.7% sulfuric acid, 0.02% zinc sulfate and 3.0% sodium sulfate, whose immersion length was 30 cm.
  • the stretchability is a value expressed in percentage of the relative peripheral speed of the second godet to that of the first godet at the time breakage of monofilaments occurs between the first and second godets when the peripheral speed of the first godet is held constant while that of the second godet is raised.
  • the spinnability is a value expressed in percentage of the ratio of the peripheral speed of the first godet to the linear speed of viscose being extruded from the spinneret at the time breakage of yarn occurs between the spinneret and the first godet when the linear speed of the viscose being extruded from the nozzle is held constant while the peripheral speed of the first godet is raised.
  • the viscose is extruded into a spinning bath containing sulfuric acid of low concentration and sulfates of low concentration while controlling the foregoing conditions.
  • concentration of the sulfuric acid is, for example, 46%
  • zinc sulfate is, for example, 0.00l1%
  • sodium sulfate is, for example, 36%.
  • temperature of the spinning bath is preferably within a range of 3060 C. A ratio of stretching of, say, 1.21.8 is desirable in this invention.
  • viscose rayon filaments of excellent touch and good luster and having high wet modulus can be spun at a high speed of such as at least 80 meters per minute, employing a horizontal type spinning machine, for example, the Topham type spinning machine.
  • the spinning can moreover be raised readily to as high as, say, about 180 meters per minute, and fibers having fully satisfactory properties can be obtained at such a speed.
  • This invention is applicable to monofilaments of, say, 0.7 .0 deniers and a wide range of total deniers of such, for example, as 30-1000 deniers.
  • a wide range of total deniers of such for example, as 30-1000 deniers.
  • Example 1 Alkali cellulose obtained by steeping pulp in an alkali and crushing was aged for 2 hours at 25 (3., following which 45% of carbon disulfide was added based on the cellulose followed by reacting for 3 hours at 25 C. and thereafter the cellulose xanthate was dissolved in a dilute alkali. Holding the total alkali content at 3.75%, three classes of viscose were thus prepared whose cellulose contents were respectively 4.1%, 5.0% (present invention) and 6.0%. A fourth class was also prepared in which the cellulose content was 5 .0%, while the total alkali content was 3.24%. The average degree of polymerization of the viscose was 520 in all four instances.
  • EXAMPLE 2 Alkali cellulose obtained by steeping pulp in an alkali and crushing was ripened for 2 hours, after which 46% of carbon disulfide based on the cellulose was added thereto followed by reacting for 3 hours at 25 C.
  • Three classes of viscose were prepared by dissolving the cellulose xanthate in a dilute alkali, adjusting the cellulose content to a constant value of 4.5% while varying the total alkali contents respectively to 3.15%, 3.42% and 4.5
  • the degree of polymerization of the viscose was 520 in all three instances.
  • EXAMPLE 5 Viscose having a cellulose content of 5.0%, a total alkali content of 3.75% and a degree of polymerization of 520, as obtained in Example 1, immediately prior to its being spun with a horizontal Topham type spinning machine, was heated at 45 C. (present invention), 35 C. (present invention), or not heated, following which the spinning was carried out at the spinning speeds of 125, 150 and 170 meters per minute.
  • the properties of the yarn so obtained are shown in Table V. In this case, excepting for the sulfuric acid concentration of the spinning bath, the spinning conditions were otherwise identical to those of Example 1. The sulfuric acid concentrations were as indicated in Table V.
  • a method of spinning viscose rayon filaments having a high wet modulus at high speeds which comprises heating of viscose at 3560 C. the viscose having a degree of polymerization ranging between 400 and 700 and a gamma value at the time of spinning of 6580, and in which the relationship between the degree of polymerization, cellulose content and total alkali content of said viscose satisfies the following Formulae 1 and 2 wherein D1 is the average degree of polymerization, CC is the cellulose content of the viscose in percent and TA is the total alkali content of the viscose in percent, said TABLE V Spinning speed m./min 125 Viscose heating temperature, C 35 Concentration of sulfuric acid,
  • Viscose having a cellulose content of 4.5%, a total alkali content of 3.42% and a degree of polymerization of 520 as obtained in Example 2, immediately prior to its being spun with a horizontal Topham type spinning maheating being effected immediately prior to the spinning of said viscose, followed by extruding said viscose into a single spinning bath containing 46% by weight of sulfuric acid, 36% by weight of sodium sulfate and 0.001 0.1% by Weight of zinc sulfate, with the temperature of said bath being maintained at 30-60 C.
  • ning being eifected at a spinning speed of at least 80 meters per minute using a horizontal type spinning machine.

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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)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
US660419A 1967-08-14 1967-08-14 High speed spinning method of viscose rayon filaments having high wet modulus Expired - Lifetime US3539678A (en)

Applications Claiming Priority (7)

Application Number Priority Date Filing Date Title
US66041967A 1967-08-14 1967-08-14
GB37432/67A GB1171839A (en) 1967-08-14 1967-08-15 High Speed Spinning Viscose Rayon Filaments having High Wet Modulus.
CH1186967A CH503808A (de) 1967-08-14 1967-08-24 Verfahren zur Herstellung von Viskosekunstseidefilamenten von hohem Nassmodul
BE703189 1967-08-28
FR119857 1967-09-04
NL6712159A NL6712159A (xx) 1967-08-14 1967-09-05
DET0034736 1967-09-07

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US3539678A true US3539678A (en) 1970-11-10

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US (1) US3539678A (xx)
BE (1) BE703189A (xx)
CH (1) CH503808A (xx)
DE (1) DE1669547A1 (xx)
FR (1) FR1548420A (xx)
GB (1) GB1171839A (xx)
NL (1) NL6712159A (xx)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6538130B1 (en) * 1997-09-23 2003-03-25 Acordis Kelheim Gmbh Manufacture of viscose and of articles therefrom
WO2009089556A1 (en) 2008-01-16 2009-07-23 Lenzing Ag Fibre blends, yarns and fabrics made thereof
US20100190891A1 (en) * 2007-05-09 2010-07-29 Borealis Technology Oy Polyefin compositions with highly crystalline cellulose regenrate fibers
US20100291823A1 (en) * 2008-01-11 2010-11-18 Lenzing Ag Microfiber
WO2013020150A1 (de) 2011-08-10 2013-02-14 Lenzing Ag Aktivkohle-enthaltende cellulosische man-made faser sowie verfahren zu deren herstellung und verwendung

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2307863A (en) * 1940-12-03 1943-01-12 Du Pont Spinning of artificial filaments
US2611928A (en) * 1948-11-23 1952-09-30 American Viscose Corp Method for producing high tenacity artificial yarn and cord
US2954270A (en) * 1955-12-14 1960-09-27 Chimiotex Sa Process of producing a shrinkable cellulose textile filament
GB994613A (en) * 1962-12-27 1965-06-10 Tachikawa Res Inst Improvements in or relating to the manufacture of regenerated cellulose filaments
US3324216A (en) * 1962-05-16 1967-06-06 Toyo Spinning Co Ltd Viscose spinning process

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2307863A (en) * 1940-12-03 1943-01-12 Du Pont Spinning of artificial filaments
US2611928A (en) * 1948-11-23 1952-09-30 American Viscose Corp Method for producing high tenacity artificial yarn and cord
US2954270A (en) * 1955-12-14 1960-09-27 Chimiotex Sa Process of producing a shrinkable cellulose textile filament
US3324216A (en) * 1962-05-16 1967-06-06 Toyo Spinning Co Ltd Viscose spinning process
GB994613A (en) * 1962-12-27 1965-06-10 Tachikawa Res Inst Improvements in or relating to the manufacture of regenerated cellulose filaments

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6538130B1 (en) * 1997-09-23 2003-03-25 Acordis Kelheim Gmbh Manufacture of viscose and of articles therefrom
US20100190891A1 (en) * 2007-05-09 2010-07-29 Borealis Technology Oy Polyefin compositions with highly crystalline cellulose regenrate fibers
US20100291823A1 (en) * 2008-01-11 2010-11-18 Lenzing Ag Microfiber
US20150159302A1 (en) * 2008-01-11 2015-06-11 Lenzing Ag Microfiber
US11932969B2 (en) * 2008-01-11 2024-03-19 Lenzing Aktiengesellschaft Microfiber
WO2009089556A1 (en) 2008-01-16 2009-07-23 Lenzing Ag Fibre blends, yarns and fabrics made thereof
US20110045728A1 (en) * 2008-01-16 2011-02-24 Lenzing Ag Fiber Blends, Yarns And Fabrics Made Thereof
WO2013020150A1 (de) 2011-08-10 2013-02-14 Lenzing Ag Aktivkohle-enthaltende cellulosische man-made faser sowie verfahren zu deren herstellung und verwendung

Also Published As

Publication number Publication date
CH503808A (de) 1971-02-28
FR1548420A (xx) 1968-12-06
NL6712159A (xx) 1969-03-07
GB1171839A (en) 1969-11-26
BE703189A (xx) 1968-01-15
DE1669547A1 (de) 1970-12-03

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