US3038778A - Manufacture of viscose rayon - Google Patents

Manufacture of viscose rayon Download PDF

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Publication number
US3038778A
US3038778A US740189A US74018958A US3038778A US 3038778 A US3038778 A US 3038778A US 740189 A US740189 A US 740189A US 74018958 A US74018958 A US 74018958A US 3038778 A US3038778 A US 3038778A
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United States
Prior art keywords
bath
threads
temperature
viscose
stretch
Prior art date
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
Application number
US740189A
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English (en)
Inventor
Berthold H Daimler
Elling Hugo
Elssner Richard
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Akzona Inc
Original Assignee
American Enka Corp
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Publication date
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Publication of US3038778A publication Critical patent/US3038778A/en
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    • D—TEXTILES; PAPER
    • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
    • D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
    • D02J1/223—Stretching in a liquid bath
    • 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
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
    • 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

  • the present invention relates to the manufacture of viscose rayon and more particularly to a process for producing high strength viscose rayon wherein the stretch tension of freshly spun viscose rayon threads is lowered and the stretchability of such threads is increased.
  • viscose solution is extruded through a spinneret into a coagulating and regenerating bath comprising an aqueous acid solution and containing sulfate salts.
  • a spinneret In order to obtain threads having high strength, it is necessary to subject the freshly spun threads to strong stretching after coagulation but before complete regeneration thereof. Generally, the strength increases in direct proportion to the increase in stretch.
  • the conventional system used to impart a strong stretch to freshly spun threads is known as the two-bat spinning process which includes the aforesaid coagulating and regenerating bath and a second stretch bath that is maintained at a high temperature, for example, in the range from 50 to 90 C. At this temperature the threads during their passage through the second bath are capable of accepting a high degree of stretch Without rupture.
  • the second bath usually is composed of a dilute acid solution but may be alkaline, in which case the alkaline bath may also contain compounds of zinc or aluminum.
  • the stretch is limited to a fixed value for a given set of spinning conditions and cannot exceed the breaking point of the thread.
  • stretching exceeds this point the broken threads cause entanglement and the threads so produced have an undesirable fibrous character. Consequently, it would be advantageous to increase the stretchability of freshly spun viscose threads without causing thread breakage. 7 An increase in such stretchability would be indicated either by being able to stretch eyond the normal breaking point of the threads or by achieving a lowering of the tension necessary to impart a given stretch to the threads.
  • Another object is to provide an improved process in which the stretchability of freshly spun regenerated cellulose threads from viscose is increased.
  • a further object is to provide an improved process in which freshly spun regenerated cellulose threads from viscose exhibit an increased stretchability in a hot second stretch bath.
  • Such salts include sodium sulfate and zinc sulfate.
  • a notable and further improvement in the strength value of the threads is obtained by maintaining the acid concentration in the cold intermediate bath within the range of 10 to 40 grams of acid per kilogram of the bath. It is highly important to avoid the use of a high acid concentration in the intermediate bath, because at high acid concentrations, any lowering of tension induced by the washing of the thread would be cancelled.
  • the preferred acid concentration depends on the spinning conditions with optimum results being obtained when the liquid in the threads after leaving the intermediate bath but before same enters the hot second bath has an acid content of 2 to 30 grams per kilogram, preferably 5 to 20 grams per kilogram.
  • the temperature of the intermediate bath be below 40 0., because above this temperature stretchability of the threads is reduced.
  • the reduced stretchability may be attributed to the fact that at temperatures above 40 C. the regeneration of the cellulose is accelerated.
  • the minimum temperature necessary to obtain the enhanced stretchability of the present invention is about 15 C. below this temperature one does not attain any additional substantial increase in stretchability.
  • the preferred temperature range is between 20 and 30 C.
  • the spinbath contained 40 grams of H per kilogram of bath, 120 grams of Na SO per kilogram of bath, and 50 grams of ZnSO per kilogram of bath, and had a temperature of 40 C.
  • the length of thread immersion in the spinbath was 70 cm.
  • the threads were withdrawn from the bath and passed through a cold intermediate bath for a distance of 25 cm.
  • a deflecting roller associated with a first withdrawal system and which ran in a tray through which the intermediate bath flowed was used.
  • the temperature of the intermediate bath was 25 C. After the threads were withdrawn from the intermediate bath, they were stretched 100% in a conventional hot second stretch bath.
  • EXAMPLE II A viscose solution having the composition of 6.1% cellulose and 4.2% alkali and a xanthate ratio of 43 was extruded through a spinneret having 1000 orifices into an aqueous coagulating and regenerating spinbath. Each kilogram of the viscose solution contained 0.2 gram of the amine described in Example I. The spinbath contained 30 grams of H 50 per kilogram of bath, 200 grams of Na SO per kilogram of bath, and 70 grams of ZnSO per kilogram of bath, and had a temperature of 55 C. The length of thread immersion in the spinbath was 35 cm.
  • the threads were withdrawn from the spinbath and passed directly in a hot second stretch bath where the threads were stretched 85%.
  • the thread immersion in the second bath was 180 cm.
  • the stretch tension required to impart such stretch was 1500 grams.
  • the intermediate bath was contained in a small trough and was constantly supplied thereto from a larger storage container, with the bath being discharged and returned to the container.
  • the intermediate bath was necessary to reject a certain quantity of the used bath continuously and replace it with fresh bath.
  • a process for producing high strength viscose threads comprising extruding a viscose solution into an aqueous acidic coagulating and regenerating first bath containing salts to form viscose threads therefrom, withdrawing the thus-formed threads from said first bath, passing said threads through a cold aqueous intermediate bath maintained at a temperature of 1535 C. but substantially lower than the temperature of said first bath, whereby the salt content of the liquid entrained in said threads is reduced by their contact with said intermediate bath, and passing said threads into a hot second bath maintained at a temperature substantially higher than the temperature of said first bath wherein said threads are given a substantial stretch.
  • a process for producing high strength viscose threads comprising extruding a viscose solution into an aqueous acidic coagulating and regenerating first bath containing salts to form viscose threads therefrom, withdrawing the thus-formed threads from said first bath, passing said threads through a cold aqueous intermediate bath containing a small amount of sulfuric acid and maintained at a temperature of 15-35 C. but substantially lower than the temperature of said first bath, whereby the salt content of the liquid entrained in said threads is reduced by their contact with said intermediate bath, and passing said threads into a hot second bath maintained at a temperature substantially higher than the temperature of said first bath wherein said threads are given a substantial stretch.
  • a process for producing high strength viscose threads comprising extruding a viscose solution into an aqueous acidic coagulating and regenerating first bath containing salts to form viscose threads therefrom, withdrawing the thus-formed threads from said first bath, passing said threads through a cold aqueous intermediate bath containing -40 grams of sulfuric acid per kilogram of intermediate bath and maintained at a temperature of -35 C. but substantially lower than the temperature of said first bath, whereby the salt content of the liquid entrained in said threads is reduced by their contact with said intermediate bath, and passing said threads into a hot second bath maintained at a temperature substantially higher than the temperature of said first bath wherein said threads are given a substantial stretch.
  • a process for producing high strength viscose threads comprising extruding a viscose solution into an aqueous acidic coagulating and regenerating first bath containing salts to form viscose threads therefrom, withdrawing the thus-formed threads from said first bath, passing said threads through a cold aqueous intermediate bath containing 10-40 grams of sulfuric acid per kilogram of intermediate bath and maintained at a temperature of -30 C. but substantially lower than the temperature of said first bath, whereby the salt content of the liquid entrained in said threads is reduced by their contact with said intermediate bath, and passing said threads into a hot second bath maintained at a tempera ture substantially higher than the temperature of said first bath wherein said threads are given a substantial stretch.
  • a process to; producing high strength viscose threads comprising extruding a viscose solution into an aqueous acidic coagulating and regenerating first bath containing salts to form viscose threads therefrom, withdrawing the thus-formed threads from said first bath, passing said threads through a cold aqueous intermediate bath containing 10-40 grams of sulfuric acid per kilogram of intermediate bath and formaldehyde and maintained at a temperature of 15-35 C. but substantially lower than the temperature of said first bath, whereby the salt content of the liquid entrained in said threads is reduced by their contact with said intermediate bath, and passing said threads into a hot second bath maintained at a temperature substantially higher than the temperature of said first bath wherein said threads are given a substantial stretch.
  • a process for producing high strength viscose threads comprising extruding a viscose solution into an aqueous coagulating and regenerating first bath containing sulfuric acid, sodium sulfate and zinc sulfate to form viscose threads therefrom, withdrawing the thus-formed threads from said first bath, passing said threads through a cold aqueous intermediate bath containing 10-40 grams of sulfuric acid per kilogram of intermediate bath and maintained at a temperature of 20-30" C.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
US740189A 1957-06-21 1958-06-06 Manufacture of viscose rayon Expired - Lifetime US3038778A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEV12634A DE1058692B (de) 1957-06-21 1957-06-21 Verfahren zur Erniedrigung der Streckenspannung bzw. zur Erhoehung der Verstreckbarkeit von frisch gesponnenen Faeden nach dem Viskosespinnverfahren

Publications (1)

Publication Number Publication Date
US3038778A true US3038778A (en) 1962-06-12

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US740189A Expired - Lifetime US3038778A (en) 1957-06-21 1958-06-06 Manufacture of viscose rayon

Country Status (7)

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US (1) US3038778A (xx)
BE (1) BE567067A (xx)
CH (1) CH347600A (xx)
DE (1) DE1058692B (xx)
FR (1) FR1195060A (xx)
GB (1) GB854152A (xx)
NL (1) NL227978A (xx)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3277226A (en) * 1962-04-09 1966-10-04 Fmc Corp Viscose rayon fiber and method of making same
US3351696A (en) * 1960-04-22 1967-11-07 Cta Cie Ind De Textiles Artifi Method for producing regenerated cellulose products
US3539679A (en) * 1965-08-03 1970-11-10 Mitsubishi Rayon Co Process for producing polynosic fibers

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB993786A (en) * 1960-10-04 1965-06-02 Toho Rayon Kk Process for the manufacture of high tenacity viscose rayon
BE756032A (fr) * 1969-09-12 1971-02-15 Mitsubishi Rayon Co Procede de preparation d'un produit fibreux non tisse

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2192074A (en) * 1935-12-12 1940-02-27 Courtaulds Ltd Manufacture and production of artificial threads, filaments, and the like by the viscose process
US2297613A (en) * 1938-11-09 1942-09-29 Walther H Duisberg Process of producing viscose rayon
US2327516A (en) * 1939-07-22 1943-08-24 Fink Heinrich Manufacture of artificial filaments and fibers from viscose
US2452130A (en) * 1943-12-17 1948-10-26 American Enka Corp Method of spinning high tenacity viscose rayon
US2882122A (en) * 1956-01-05 1959-04-14 Du Pont Process for producing crimpable regenerated cellulose filaments

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR885986A (fr) * 1941-09-20 1943-09-30 Zellwolle Kunstseide Ring Gmbh Procédé de fabrication de produits synthétiques tels que fils, fibres, rubans, pellicules, etc. à partir de la cellulose régénérée, et plus spécialement d'après le procédé de la viscose
BE455878A (xx) * 1943-03-26 1944-06-30
AT169926B (de) * 1946-11-26 1951-12-27 Onderzoekings Inst Res Verfahren zur Herstellung von Viskose-Kunstseide mit sehr hoher Festigkeit

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2192074A (en) * 1935-12-12 1940-02-27 Courtaulds Ltd Manufacture and production of artificial threads, filaments, and the like by the viscose process
US2297613A (en) * 1938-11-09 1942-09-29 Walther H Duisberg Process of producing viscose rayon
US2327516A (en) * 1939-07-22 1943-08-24 Fink Heinrich Manufacture of artificial filaments and fibers from viscose
US2452130A (en) * 1943-12-17 1948-10-26 American Enka Corp Method of spinning high tenacity viscose rayon
US2882122A (en) * 1956-01-05 1959-04-14 Du Pont Process for producing crimpable regenerated cellulose filaments

Cited By (3)

* 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
US3277226A (en) * 1962-04-09 1966-10-04 Fmc Corp Viscose rayon fiber and method of making same
US3539679A (en) * 1965-08-03 1970-11-10 Mitsubishi Rayon Co Process for producing polynosic fibers

Also Published As

Publication number Publication date
FR1195060A (fr) 1959-11-13
CH347600A (de) 1960-07-15
NL227978A (xx)
BE567067A (xx)
DE1058692B (de) 1959-06-04
GB854152A (en) 1960-11-16

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