US3139467A - Method for spinning viscose - Google Patents

Method for spinning viscose Download PDF

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Publication number
US3139467A
US3139467A US237527A US23752762A US3139467A US 3139467 A US3139467 A US 3139467A US 237527 A US237527 A US 237527A US 23752762 A US23752762 A US 23752762A US 3139467 A US3139467 A US 3139467A
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United States
Prior art keywords
filaments
bath
viscose
spinning
cellulose
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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US237527A
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English (en)
Inventor
Drisch Nicolas
Herrbach Paul
Rodier Henri
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Chimiotex SA
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Chimiotex
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Publication date
Priority to BE624034D priority Critical patent/BE624034A/xx
Priority to FR871410A priority patent/FR1308605A/fr
Application filed by Chimiotex filed Critical Chimiotex
Priority to US237527A priority patent/US3139467A/en
Application granted granted Critical
Publication of US3139467A publication Critical patent/US3139467A/en
Anticipated expiration legal-status Critical
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet spinning methods
    • 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

  • This invention relates to a viscose spinning process and has for an object the manufacture of fibers, filaments, etc., having high mechanical characteristics and with stable microfibrillar structure, belonging notably to the group of polynosics.
  • the filaments on coming out of the bath are supported on a partially immersed roll.
  • the chemistry of the viscose and of the bath notably the degree of sulfocarbona'tion of the viscose and the acid concentration must be suitably controlled.
  • the filaments barely coagulated'by a cold bath with very low acid concentration and incapable of continuing by themselves, are supported on coming out of the bath by a partially immersed roll having the same peripheral speed as the feed speed of the filaments, the point of tangency of the filaments with the roll being approximately at the level of the bath.
  • the filaments When they have covered a certain distance on the outer part of the roll, coagulation has sufficiently progressed and the filaments then have sufilcient strength to be able to continue by themselves in the air and to be subjected to stretching operations. Consequently, the bath adhering to the filaments continues to be neutralized on the course over the outer part of the roll and when the filaments have acquired enough strength to undergo stretching, they are impregnated in a weaker acid bath. As a result, at that time the pH of the gel may be neutral, or even alkaline.
  • the quantity of bath still adhering to the filaments can moreover 3,139,467 Patented June 30., 1964 also be controlled, by submitting the gel on the roll to slight drying by means of a force pump the pressure of which is regulated.
  • filaments which necessarily have sutficient strength on coming out of the bath to be able to continue in the air are not only in a more advanced state of regeneration, but, moreover, are still impregnated with the bath which is relatively more concentrated and, consequently causes regeneration to continue.
  • the viscose is brought through swan neck 4- to spinneret 1 and the filaments 5 formed in spinning bath 2 are directed over partially immersed roll 3 so that point of tangency A is situated on level N of the spinning bath.
  • the filaments are supported by roll 3 up to point B where the pressure of a roll 6 is exerted and the filaments then pass in succession over rolls 7, 8, 9, 10, 11 between which they are subjected to gradually increasing stretching. They are then picked up by rolls 12, pass into second bath 13, over rolls 14 and 15 and, finally, are wound on spool 16.
  • the roll 3 may be finely perforated on its cylindrical surface and provided with an inner screen 17 on its immersed part, so as to be able to eliminate through suction part of the liquid impregnating the filaments which are in gel state.
  • the degree of immersion of roll 3 and the angle of contact of filaments 5 on this roll are not critical and can be varied. It is, however, important that the point of tangency A not be situated above the level N of the bath so that the filaments are brought into contact and are supported by the roll 3 before they leave the bath.
  • gammas in the order of 50 can be attained at point B, i.e., at the start of stretching, and stretching can be easily completed at a gamma ranging between 10 and 20.
  • This process makes it possible to spin at very low acidities (15 g./liter and less), with spinnerets having a large number of holes (8,000 to 15,000, for example). It is suitable for the manufacture of polynosic fibers.
  • the process is also usable, however, for the spinning of textile rayon and tire rayon. In the latter case, primary stretching is markedly reduced in order to provide for greater stretch in the second bath.
  • the gel is picked up in the desired place and is imme diately centrifuged at 300 G. for 5 minutes at low temperature. A quantity of 25 g. of this centrifuged gel is then introduced into 750 cc. of distilled ice water and, after stirring, the pH of the extraction water is measured. A conventional figure is obtained which is a measure of the state of decomposition of the gel.
  • Table 1 gives, for example: For a 5.2/3.8 viscose and 3 different baths, the pH of gels which have been obtained after roll 3 (point B), as a function of vertical travel in Bath, HZSOl/SOJNEZ, 15-35 g./l., Temperature 20 C 2 1. 3 l. 1 Bath, H2SOi/SO4Na2, 15-35 g./l., Temperature 10 C 7. 1 6 5.
  • the pH and gamma index of the gel can be further controlled.
  • the following figures were obtained, as indicated in Table 3:
  • a viscose containing at least 3% cellulose and from 1.5 to 10% soda the sulforcarbonation rate of which is at least in relation to the alpha-cellulose can be used.
  • the gamma index of the viscose used in spinning should have a range between and 100 and the cellulose contained in the viscose should have a DP of at least 500 and preferably above 600.
  • the viscosity of the viscose at time of spinning should range between 150 and 1000 poises and is preferably above 400 poises.
  • the viscose is spun in a bath containing less than 60 g./l., preferably, 8 to 40 g./l., sulfuric acid, 10 to 120 g./l., sodium sulfate and no or little (less than 1%) zinc sulfate.
  • the bath can further contain small quantities of formal or a modifying agent such as polyalkylene oxide.
  • the temperature of the bath ranges between 0 and 40 C., preferably between 5 and 30 C.
  • the filaments obtained are stretched at least 100% and preferably at least 160%, which stretching can be imparted during travel in the air between the two baths and/or in a second hot dilute acid bath.
  • the yarn is preferably collected on spools. If staple fiber is spun, the roving is passed in slack state to a third degassing bath and is then placed in cans.
  • Filaments manufactured according to the present process have a high strength exceeding 4.5 g./den. in conditioned state and 4 g./den. in wet state and also a high modulus of elasticity in wet state, having an elongation in wet state of less than 3% under a load of 0.5 g./d. They are circular in section and their swelling is less than
  • nitric acid it can be verified that the filaments in question possess a highly characteristic fibrillar structure far closer to that of cotton than to that of other regenerated cellulose yarns.
  • Physical testing as, for example, X-ray diagram and double refraction determination, reveal the existence of an extremely oriented structure.
  • the filaments just described After treatment with 5% soda, the filaments just described still have a strength of wet state of 4 g./den. and a modulus in wet state (elongation percent under 0.5 g./den. of 3.
  • Example 2 Wood pulp having a high alpha-cellulose content is converted into alkali cellulose and the latter is immediately sulfocarbonated without any intermediate ripening with 57% carbon disulfide in relation to alpha-cellulose; the xanthate formed is then dissolved in dilute soda to yield a 6.5 :5 viscose to which suitable surface-active products are added.
  • the DP of the cellulose contained in the viscose is 550 and the viscosity is 500 poises.
  • Viscose is spun in a vertical spinning device as described above by means of a spinneret with 40 holes of .07 mm. in a bath containing 15 g./l. sulfuric acid and 75 g./l.
  • a process for the manufacture of fibers or filaments having high mechanical characteristics, a stable microfibrillar structure and good dimensional stability which comprises spinning a viscose containing a cellulose having a DP of at least 500 and a viscosity of at least 150 poises and a gamma index of at least with a cold acid bath containing not over grams of sulfuric acid per liter and from 10 to g./l.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
US237527A 1961-08-23 1962-11-14 Method for spinning viscose Expired - Lifetime US3139467A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
BE624034D BE624034A (zh) 1962-11-14
FR871410A FR1308605A (fr) 1961-08-23 1961-08-23 Nouveau procédé de filature de la viscose et dispositif à cet effet
US237527A US3139467A (en) 1962-11-14 1962-11-14 Method for spinning viscose

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3320117A (en) * 1962-05-31 1967-05-16 Tachikawa Res Inst Process for the manufacture of rayon paper or non-woven fabric by the wet system
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
US3351696A (en) * 1960-04-22 1967-11-07 Cta Cie Ind De Textiles Artifi Method for producing regenerated cellulose products
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
US3432589A (en) * 1967-11-06 1969-03-11 Chimiotex Sa Process for manufacturing regenerated cellulose filaments
US3506754A (en) * 1967-09-27 1970-04-14 Tachikawa Res Inst Process for manufacturing rayon having high degree of polymerization by the viscose process
US3539679A (en) * 1965-08-03 1970-11-10 Mitsubishi Rayon Co Process for producing polynosic fibers
US3875141A (en) * 1968-02-16 1975-04-01 Chimiotex Regenerated cellulose filaments
US4383962A (en) * 1979-09-27 1983-05-17 Asahi Kasei Kogyo Kabushiki Kaisha Process for producing viscose rayon filament yarn
WO1998008393A1 (en) 1996-08-27 1998-03-05 Alfacel S.A. Method to slowly regenerate cellulosic sausage casing
US5813068A (en) * 1994-12-23 1998-09-29 Bayer Faser Gmbh Apparatus and a process for washing continuously wet-spun elastane
US5851290A (en) * 1994-11-02 1998-12-22 Tissue Engineering, Inc. Apparatus for spinning and processing collagen fiber
US5911942A (en) * 1995-11-02 1999-06-15 Tissue Engineering, Inc. Method for spinning and processing collagen fiber

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2705184A (en) * 1949-08-25 1955-03-29 Textile & Chemical Res Company Process for the production of rayon products
US3024493A (en) * 1958-01-30 1962-03-13 Phrix Werke Ag Adjustably shielded suction drum for circulating bath liquid

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2705184A (en) * 1949-08-25 1955-03-29 Textile & Chemical Res Company Process for the production of rayon products
US3024493A (en) * 1958-01-30 1962-03-13 Phrix Werke Ag Adjustably shielded suction drum for circulating bath liquid

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3351696A (en) * 1960-04-22 1967-11-07 Cta Cie Ind De Textiles Artifi Method for producing regenerated cellulose products
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
US3320117A (en) * 1962-05-31 1967-05-16 Tachikawa Res Inst Process for the manufacture of rayon paper or non-woven fabric by the wet system
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
US3539679A (en) * 1965-08-03 1970-11-10 Mitsubishi Rayon Co Process for producing polynosic 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
US3432589A (en) * 1967-11-06 1969-03-11 Chimiotex Sa Process for manufacturing regenerated cellulose filaments
US3875141A (en) * 1968-02-16 1975-04-01 Chimiotex Regenerated cellulose filaments
US4383962A (en) * 1979-09-27 1983-05-17 Asahi Kasei Kogyo Kabushiki Kaisha Process for producing viscose rayon filament yarn
US5851290A (en) * 1994-11-02 1998-12-22 Tissue Engineering, Inc. Apparatus for spinning and processing collagen fiber
US5813068A (en) * 1994-12-23 1998-09-29 Bayer Faser Gmbh Apparatus and a process for washing continuously wet-spun elastane
US5911942A (en) * 1995-11-02 1999-06-15 Tissue Engineering, Inc. Method for spinning and processing collagen fiber
WO1998008393A1 (en) 1996-08-27 1998-03-05 Alfacel S.A. Method to slowly regenerate cellulosic sausage casing
US5783131A (en) * 1996-08-27 1998-07-21 Alfacel S.A. Method to slowly regenerate cellulosic sausage casing
EP0923299A1 (en) * 1996-08-27 1999-06-23 Alfacel S.A. Method to slowly regenerate cellulosic sausage casing
EP0923299A4 (en) * 1996-08-27 2003-01-08 Alfacel S A PROCESS FOR SLOWLY REGENERATING THE SAUSAGE CELLULOSE SHELL

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Publication number Publication date
BE624034A (zh)

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