US3626045A - Process for making tubular filaments - Google Patents

Process for making tubular filaments Download PDF

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US3626045A
US3626045A US884808A US3626045DA US3626045A US 3626045 A US3626045 A US 3626045A US 884808 A US884808 A US 884808A US 3626045D A US3626045D A US 3626045DA US 3626045 A US3626045 A US 3626045A
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Prior art keywords
filaments
percent
weight
tubular
stretching
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US884808A
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Calvin R Woodings
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COUSTAULDS Ltd
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COUSTAULDS 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
    • 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
    • D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
    • 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
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913—Rod, strand, filament or fiber
    • Y10T428/2973—Particular cross section
    • Y10T428/2975—Tubular or cellular

Definitions

  • a controllable commercial process for producing tubular regenerated cellulose filaments comprises extruding a viscose of a specific composition and containing sodium carbonate into a sulfuric acid spin bath of a specific composition to form filaments followed by stretching of the filaments.
  • Tubular filaments with increased wet modulus and a tendency to crimp are produced by stretching the filaments by an amount approaching their breaking stretch.
  • This invention relates to a process for making tubular filaments of regenerated cellulose by the viscose process. Many such processes have been proposed in the past but tubular regenerated cellulose filaments have not been produced on a commercial scale.
  • Collapsed tubular filaments have been made commercially and a process for making them is described in our British Pat. Spec. No. 945,306. These filaments are essentially different from the filaments with which the present invention is concerned in that their walls have caved in leaving little void space and producing a flat filament having a high width to thickness ratio.
  • the object of the present invention is a controllable commercial process which is capable of producing regenerated cellulose filaments of which at least 90 percent by number in a cross section of a spun tow are tubular filaments which have not collapsed to the fiat state.
  • a process for making tubular filaments of regenerated cellulose comprises extruding a viscose containing 6.5 to 9.5 percent by weight of cellulose, 5.0 to 7.0 percent by weight of caustic soda, 3.0 to 4.0 percent by weight of sodium carbonate and 0.75 to 2.0 percent by weight of polyethylene glycol based on the weight of cellulose, and having a salt figure of 12 to 18, into a spinning bath containing 8.0 to 10.0 percent by weight of sulfuric acid, 1.0 to 3.0 percent by weight of zinc sulfate, and 20.0 to 26.0 percent by weight of sodium sulfate, and at a temperature of 25 to 45 C., to form filaments, directing the filaments along an immersion path of length 30 cm. to 185 cm., and stretching the filaments by at least 40 percent.
  • the invention includes the tubular filaments produced by this process.
  • the viscose used in the process of the invention may have a concentration of carbon disulfide of 33 to 50 percent by weight based on the weight of cellulose and a ball-fall viscosity of 30 to 180 seconds at 18 C.
  • the stretching operation preferably is carried out in a hot aqueous bath containing sulfuric acid, preferably a bath at about 95 C. and containing about 2 percent by weight of sulfuric acid. It has been found that fibers with an increased wet modulus and a tendency to crimp, with only slightly reduced tensile properties, can be obtained by stretching the filaments in the stretch bath by an amount approaching the breaking stretch of the filaments, preferably to about percent below break. in this way we have obtained tubular filaments having an initial wet modulus of up to 10.0 at 2.0 percent extension and up to 12.0 at 5.0 percent extension.
  • Staple fibers produced from the filaments of the. invention may be handled with case on cotton spinning machinery.
  • the resulting yarns are of an increased bulk compared with yarn made from solid, viscose rayon filaments and fabrics made from the yarns have a handle similar to cotton and a greater absorbency.
  • the temperature of the spin bath was 30' C. and the immersion path length was 122 cm.
  • the filaments were stretched in an aqueous stretch bath containing 2.0 percent sulfuric acid and at a temperature of C. to a total of 85 percent stretch.
  • the average properties of the filaments were as follows:
  • the accompanying drawing is a highly magnified cross-sectional view of the filament tow produced by the process of the example.
  • a process for making tubular filaments of regenerated cellulose comprising extruding a viscose containing 6.5 to 9.5 percent by weight of cellulose, 5.0 to 7.0 percent by weight of caustic soda, 3.0 to 4.0 percent by weight of sodium carbonate and 0.75 to 2.0 percent by weight of polyethylene glycol based on the weight of cellulose, and having a salt figure of 12 to 18, into a spinning bath containing 8.0 to 10.0 percent by weight of cellulose, of sulfuric acid, 1.0 to 3.0 percent by weight of zinc sulfate, and 20.0 to 26.0 percent by weight of sodium sulfate and at a temperature of 25 to 45 C., to form fila ments, directing the filaments along an immersion path of length 30 cm. to cm., and stretching the filaments by at least 40 percent.

Abstract

A controllable commercial process for producing tubular regenerated cellulose filaments comprises extruding a viscose of a specific composition and containing sodium carbonate into a sulfuric acid spin bath of a specific composition to form filaments followed by stretching of the filaments. Tubular filaments with increased wet modulus and a tendency to crimp are produced by stretching the filaments by an amount approaching their breaking stretch.

Description

United States Patent Inventor Calvin R. Woodings Nuneaton, England Appl. No. 884,808
Filed Dec. 15, 1969 Patented Dec. 7, 1971 Assignee Coustaulds Limited London, England Priority Dec. 20, 1968 Great Britain 60,676/68 PROCESS FOR MAKING TUBULAR FILAMENTS 4 Claims, 1 Drawing Fig.
US. Cl 264/54, 161/178,264/188, 264/195 lnt.Cl 1301i 3/10 Field of Search 161/178; 264/188,193, 195,41-55 References Cited UNITED STATES PATENTS 11/1938 Picard 161/178 1,464,048 8/1923 Rousset 161/178 2,476,293 7/1949 Hall et a1. 161/178 2,835,551 5/1958 Kosuge 161/178 3,156,605 11/1964 Anderer et al.. 161/178 3,318,990 5/1967 Kajitani 161/178 FOREIGN PATENTS 40-9,064 5/1965 Japan 264/188 Primary Examiner-Jay H. W00 Alwrney-Davis, Hoxie, Faithful] and Hapgood ABSTRACT: A controllable commercial process for producing tubular regenerated cellulose filaments comprises extruding a viscose of a specific composition and containing sodium carbonate into a sulfuric acid spin bath of a specific composition to form filaments followed by stretching of the filaments. Tubular filaments with increased wet modulus and a tendency to crimp are produced by stretching the filaments by an amount approaching their breaking stretch.
PATENTED on: 7197: 3.6260 45 INVENTOR CALVIN ROGER woonnmr;
DAVIS, noxn-r, FAITIIFULL & IIAPGOOI) ATTORNEY PROCESS FOR MAKING TUBULAR FllLAMENTS This invention relates to a process for making tubular filaments of regenerated cellulose by the viscose process. Many such processes have been proposed in the past but tubular regenerated cellulose filaments have not been produced on a commercial scale.
Collapsed tubular filaments, on the other hand, have been made commercially and a process for making them is described in our British Pat. Spec. No. 945,306. These filaments are essentially different from the filaments with which the present invention is concerned in that their walls have caved in leaving little void space and producing a flat filament having a high width to thickness ratio.
The object of the present invention is a controllable commercial process which is capable of producing regenerated cellulose filaments of which at least 90 percent by number in a cross section of a spun tow are tubular filaments which have not collapsed to the fiat state.
According to this invention, a process for making tubular filaments of regenerated cellulose comprises extruding a viscose containing 6.5 to 9.5 percent by weight of cellulose, 5.0 to 7.0 percent by weight of caustic soda, 3.0 to 4.0 percent by weight of sodium carbonate and 0.75 to 2.0 percent by weight of polyethylene glycol based on the weight of cellulose, and having a salt figure of 12 to 18, into a spinning bath containing 8.0 to 10.0 percent by weight of sulfuric acid, 1.0 to 3.0 percent by weight of zinc sulfate, and 20.0 to 26.0 percent by weight of sodium sulfate, and at a temperature of 25 to 45 C., to form filaments, directing the filaments along an immersion path of length 30 cm. to 185 cm., and stretching the filaments by at least 40 percent.
The invention includes the tubular filaments produced by this process.
The viscose used in the process of the invention may have a concentration of carbon disulfide of 33 to 50 percent by weight based on the weight of cellulose and a ball-fall viscosity of 30 to 180 seconds at 18 C.
The stretching operation preferably is carried out in a hot aqueous bath containing sulfuric acid, preferably a bath at about 95 C. and containing about 2 percent by weight of sulfuric acid. It has been found that fibers with an increased wet modulus and a tendency to crimp, with only slightly reduced tensile properties, can be obtained by stretching the filaments in the stretch bath by an amount approaching the breaking stretch of the filaments, preferably to about percent below break. in this way we have obtained tubular filaments having an initial wet modulus of up to 10.0 at 2.0 percent extension and up to 12.0 at 5.0 percent extension.
Staple fibers produced from the filaments of the. invention may be handled with case on cotton spinning machinery. The resulting yarns are of an increased bulk compared with yarn made from solid, viscose rayon filaments and fabrics made from the yarns have a handle similar to cotton and a greater absorbency.
The invention is illustrated by the following example in which the percentages are be weight.
EXAMPLE A viscose containing 7.0 percent cellulose, 5.5 percent caustic soda, 45 percent carbon disulfide based on the weight of cellulose, 4.0 percent sodium carbonate, and 1.0 percent polyethylene glycol, and with a salt figure of 15 and a ball-fall viscosity of 50 seconds at 18 C., was extruded into a spin bath containing 9.3 percent sulfuric acid, 2.0 percent zinc sulfate and 23 percent sodium sulfate, to form filaments of 1.5 denier.
The temperature of the spin bath was 30' C. and the immersion path length was 122 cm.
The filaments were stretched in an aqueous stretch bath containing 2.0 percent sulfuric acid and at a temperature of C. to a total of 85 percent stretch.
The average properties of the filaments were as follows:
Air dry tenacity 2.6 g. per denier Air dry extensibility 1 1.0 percent Wet extensibility l 1.0 percent Wet tenacity 1.7 g. per denier Initial Wet Modulus at 2.0 percent extension 7.6 Initial Wet Modulus at 5.0 percent extension 9.5 Water imbibition l 30 Crimp 45 waves per cm.
The accompanying drawing is a highly magnified cross-sectional view of the filament tow produced by the process of the example.
What is claimed is:
l. A process for making tubular filaments of regenerated cellulose comprising extruding a viscose containing 6.5 to 9.5 percent by weight of cellulose, 5.0 to 7.0 percent by weight of caustic soda, 3.0 to 4.0 percent by weight of sodium carbonate and 0.75 to 2.0 percent by weight of polyethylene glycol based on the weight of cellulose, and having a salt figure of 12 to 18, into a spinning bath containing 8.0 to 10.0 percent by weight of cellulose, of sulfuric acid, 1.0 to 3.0 percent by weight of zinc sulfate, and 20.0 to 26.0 percent by weight of sodium sulfate and at a temperature of 25 to 45 C., to form fila ments, directing the filaments along an immersion path of length 30 cm. to cm., and stretching the filaments by at least 40 percent.
2. A process as claimed in claim 1 in which the filaments are stretched in a hot, aqueous bath containing sulfuric acid.
3. A process as claimed in claim 1 in which the filaments are stretched by an amount approaching the stretch at which the filaments break.
4. A process as claimed in claim 3 in which the filaments are stretched by an amount which is about 10 percent below the stretch at which the filaments break.
g ggg UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No. 3,626,045 Dated December 7, 1971 Inventor-(s) CALVIN R. WOODINGS It is certified that error appears in the above-identified patent and that said Letters Patent are hereby corrected as shown below:
Col. 2, line 15, "cm. should read cms.
Claim 1, line 39, delete "of cellulose,"
line 43, "30 cm. to 185 cm." should be 30 cms. to 185 cms.
Signed and sealed this 25th day of July 1972.
(SEAL) Attest:
EDWARD M.FIETCHER,JB. ROBERT GOTTSCHALK Attesting Officer Commissioner of Patents

Claims (3)

  1. 2. A process as claimed in claim 1 in which the filaments are stretched in a hot, aqueous bath containing sulfuric acid.
  2. 3. A process as claimed in claim 1 in which the filaments are stretched by an amount approaching the stretch at which the filaments break.
  3. 4. A process as claimed in claim 3 in which the filaments are stretched by an amount which is about 10 percent below the stretch at which the filaments break.
US884808A 1968-12-20 1969-12-15 Process for making tubular filaments Expired - Lifetime US3626045A (en)

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GB60676/68A GB1283529A (en) 1968-12-20 1968-12-20 Process for making tubular filaments of regenerated cellulose

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2354400A1 (en) * 1976-06-11 1978-01-06 Int Paper Co PROCESS FOR THE PREPARATION OF HOLLOW RAYON-VISCOSE FIBERS
US4129679A (en) * 1969-11-27 1978-12-12 Courtaulds Limited Multi-limbed regenerated cellulose filaments
US4130689A (en) * 1976-06-11 1978-12-19 International Paper Company Production of high strength hollow rayon fibers
US4182735A (en) * 1978-05-25 1980-01-08 International Paper Company Production of high crimp, high strength, hollow rayon fibers
US4185059A (en) * 1976-03-10 1980-01-22 Bayer Aktiengesellschaft Process for the preparation of hydrophilic fibres and filaments from synthetic polymers
US4242411A (en) * 1978-05-25 1980-12-30 International Paper Company High crimp, high strength, hollow rayon fibers
US5124197A (en) * 1989-07-28 1992-06-23 Kimberly-Clark Corporation Inflated cellulose fiber web possessing improved vertical wicking properties
US5158844A (en) * 1991-03-07 1992-10-27 The Dexter Corporation Battery separator
US5634914A (en) * 1987-07-30 1997-06-03 Courtaulds Plc Cellulosic fibre
US20080090076A1 (en) * 2004-12-10 2008-04-17 Lenzing Aktiengesellschaft Cellulosic staple fiber and its use
US20090020247A1 (en) * 2002-09-13 2009-01-22 Agne Swerin Paper with improved stiffness and bulk and method for making same
US20100051220A1 (en) * 2008-08-28 2010-03-04 International Paper Company Expandable microspheres and methods of making and using the same
US8317976B2 (en) 2000-01-26 2012-11-27 International Paper Company Cut resistant paper and paper articles and method for making same
US8377526B2 (en) 2005-03-11 2013-02-19 International Paper Company Compositions containing expandable microspheres and an ionic compound, as well as methods of making and using the same

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ATE136808T1 (en) * 1992-06-25 1996-05-15 Saechsische Kunstseiden Gmbh METHOD FOR INCREASING THE SHAPE AND SPINNING STABILITY OF CAPILLARY HOLLOW MEMBRANES

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1464048A (en) * 1921-10-13 1923-08-07 Rousset Jules Artificial textile filament and process of making same
US2136463A (en) * 1934-05-24 1938-11-15 Alsa In Basle Soc Method of preparing tubular artificial textile threads
US2476293A (en) * 1944-10-03 1949-07-19 American Viscose Corp Artificial fiber
US2835551A (en) * 1955-04-09 1958-05-20 Toyo Rayon Co Ltd Process for producing hollow viscose filaments
US3156605A (en) * 1960-03-25 1964-11-10 Fmc Corp Regenerated cellulose fiber
US3318990A (en) * 1962-08-18 1967-05-09 Kurashiki Rayon Co Method of manufacturing flat viscose fibers

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1464048A (en) * 1921-10-13 1923-08-07 Rousset Jules Artificial textile filament and process of making same
US2136463A (en) * 1934-05-24 1938-11-15 Alsa In Basle Soc Method of preparing tubular artificial textile threads
US2476293A (en) * 1944-10-03 1949-07-19 American Viscose Corp Artificial fiber
US2835551A (en) * 1955-04-09 1958-05-20 Toyo Rayon Co Ltd Process for producing hollow viscose filaments
US3156605A (en) * 1960-03-25 1964-11-10 Fmc Corp Regenerated cellulose fiber
US3318990A (en) * 1962-08-18 1967-05-09 Kurashiki Rayon Co Method of manufacturing flat viscose fibers

Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4129679A (en) * 1969-11-27 1978-12-12 Courtaulds Limited Multi-limbed regenerated cellulose filaments
US4185059A (en) * 1976-03-10 1980-01-22 Bayer Aktiengesellschaft Process for the preparation of hydrophilic fibres and filaments from synthetic polymers
FR2354400A1 (en) * 1976-06-11 1978-01-06 Int Paper Co PROCESS FOR THE PREPARATION OF HOLLOW RAYON-VISCOSE FIBERS
US4130689A (en) * 1976-06-11 1978-12-19 International Paper Company Production of high strength hollow rayon fibers
US4182735A (en) * 1978-05-25 1980-01-08 International Paper Company Production of high crimp, high strength, hollow rayon fibers
US4242411A (en) * 1978-05-25 1980-12-30 International Paper Company High crimp, high strength, hollow rayon fibers
US5634914A (en) * 1987-07-30 1997-06-03 Courtaulds Plc Cellulosic fibre
US6333108B1 (en) 1987-07-30 2001-12-25 Acordis Kelheim Gmbh Cellulose fibre compositions
US5124197A (en) * 1989-07-28 1992-06-23 Kimberly-Clark Corporation Inflated cellulose fiber web possessing improved vertical wicking properties
US5158844A (en) * 1991-03-07 1992-10-27 The Dexter Corporation Battery separator
US8317976B2 (en) 2000-01-26 2012-11-27 International Paper Company Cut resistant paper and paper articles and method for making same
US20090020247A1 (en) * 2002-09-13 2009-01-22 Agne Swerin Paper with improved stiffness and bulk and method for making same
US8460512B2 (en) 2002-09-13 2013-06-11 International Paper Company Paper with improved stiffness and bulk and method for making same
US8790494B2 (en) 2002-09-13 2014-07-29 International Paper Company Paper with improved stiffness and bulk and method for making same
US20080090076A1 (en) * 2004-12-10 2008-04-17 Lenzing Aktiengesellschaft Cellulosic staple fiber and its use
US8377526B2 (en) 2005-03-11 2013-02-19 International Paper Company Compositions containing expandable microspheres and an ionic compound, as well as methods of making and using the same
US20100051220A1 (en) * 2008-08-28 2010-03-04 International Paper Company Expandable microspheres and methods of making and using the same
US8382945B2 (en) 2008-08-28 2013-02-26 International Paper Company Expandable microspheres and methods of making and using the same
US8679294B2 (en) 2008-08-28 2014-03-25 International Paper Company Expandable microspheres and methods of making and using the same

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Publication number Publication date
FR2026714A1 (en) 1970-09-18
GB1283529A (en) 1972-07-26

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