US3046082A - Viscose process for the manufacture of low-shrink rayon - Google Patents

Viscose process for the manufacture of low-shrink rayon Download PDF

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Publication number
US3046082A
US3046082A US78779A US7877960A US3046082A US 3046082 A US3046082 A US 3046082A US 78779 A US78779 A US 78779A US 7877960 A US7877960 A US 7877960A US 3046082 A US3046082 A US 3046082A
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United States
Prior art keywords
filaments
viscose
rayon
bath
shrink
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Expired - Lifetime
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US78779A
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English (en)
Inventor
Mitchell Reid Logan
Delmont K Smith
Ralph C Welton
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Rayonier Inc
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Rayonier Inc
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Priority to NL272684D priority Critical patent/NL272684A/xx
Application filed by Rayonier Inc filed Critical Rayonier Inc
Priority to US78779A priority patent/US3046082A/en
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Expired - Lifetime legal-status Critical Current

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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
    • D02J1/228—Stretching in two or more steps, with or without intermediate steps
    • 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
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/04—Supporting filaments or the like during their treatment
    • D01D10/049—Supporting filaments or the like during their treatment as staple fibres
    • 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
    • D01D5/12—Stretch-spinning methods
    • D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
    • 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
    • D01D5/26—Formation of staple fibres
    • 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
    • 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

Definitions

  • This invention relates to the viscose process, and has for its object the provision of an improved regenerated filament and staple fiber from which low-shrinking fabrics can be formed, and an improved process for producing the filaments and staple fibers.
  • the invention produces regenerated cellulose filaments (known as rayon) that shrink less than cotton which may be considered practically shrink-free only after sanforia ng. This is accomplished without sacrificing the desirable qualities of rayon, such as high strength, flex and abrasion toughness,
  • the invention is carried out by the spinning of viscose under conditions which result in filaments having an appreciable amount of skin, most advantageously by producing filaments which are nearly or entirely allskin, and to this end the spinning is under preferred conditions of retarded regeneration needed to produce the desired skin effect.
  • the viscose filaments are spun into an acid regenerating bath and are subjected as soon as possible to a primary stretch of at least 90%, preferably a multistage stretch while in contact with strong acid spin bath carryover, at a preferred temperature of from to 70 C., and the filaments are then subjected to a secondary stretch of at least 20% in a dilute acid bath to complete regeneration.
  • the completely regenerated filamenfs are subject to a relaxation treatment in a suitable liquid medium which causes the filaments to swell, such as by immersion in a hot dilute alkaline solution of sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate, sodium sulfide, or potassium thiocyanate.
  • This relaxation treatment accompanied by the entire controlled and progressive stretching, removes any internal structural imbalances that would contribute to the capacity of the filaments to shrink in water as in laundering.
  • staple fibers are to be formed which is an important variation ofrthe invention, the regenerated filaments prior to Washing are cut into staple fibers and the mass of such fibers is washed and then immersed, preferably in a hot dilute solution of sodium hydroxide for a shorttime.
  • a preferred treatment is to immerse the fibers in an aqueous solution containing about 1% sodium hydroxide at about 90 C. for a short time, say, about one to five minutes, and then wash and finish the filaments in the conventional manner.
  • any suitable viscose composition in any of the Well known procedures for forming rayon filaments having a structure that is substantially all-skin.
  • the types of acid regenerating spin baths widely used are satisfactory such as a modified Mueller bath, preferably under conditions when either the viscose or the spin bath contains an active regeneration retardant to insure the formation of an effective high proportion of skin.
  • cellulose xanthate having a uniform chain length at a degree of polymerization of from 300 to 800, derived from such cellulose as, for example, Rayocord-X, Cordenier-J, Cor denier-X, of Rayonier Incorporated, or other high-alpha cellulose pulps, prehydrolyzed kraft, cotton linters, resinfree pulp, cold-caustic refined pulp, high purity pulp of a high degree of polymerization (DP) and uniform chain length, and preoxidized pulp of high purity low DP and uniform chain length.
  • DP degree of polymerization
  • the process may be carried out with conventional viscose compositions comprising about 7.5% of cellulose and 6.5% of sodium hydroxide, or in any suitable proportions of cellulose to sodium hydroxide varying from 4% to 13% of cellulose and from 5% to 13% of sodium hydroxide such as the following:
  • the viscose solution may be prepared according to the usual practice to have a salt (sodium chloride) index varying from 4 to 20, by xanthating the alkali cellulose with the desired amount of carbon bisulfide, say, about of the bisulfide.
  • the spinning operation is carried out in the process and a suitable acid bath to stretch the filaments initially while in contact with the spin bath at least preferaby about but usually not over about Then the filaments are led into a dilute hot acid. bath containing from 1-6%, preferably about 4%, of sulfuric acid at from 80 C. to 100 0, preferably about 90 C., to stretch them an additional 5% to 50%, preferably about 30%, to fix the crystal structure and to complete regeneration.
  • This dilute hot bath is uesd to dilute the filament salt content to permit further stretch and to decompose and remove the last traces of xanthates. It merely tolerates the adhering or residual salts from the primary spin bath as the important agent is the hot dilute sulfuric acid.
  • the regenerated filaments may be superficially washed with hot water and subjected to the relaxation treatment. After washing they may be cut into staple fibers, opened,
  • the swelling agent for example dilute caustic solution containing from 0.1% to 2%, preferably about 1%, of sodium hydroxide, at a temperature varying from 80 C. to 100 C. for a short time, say, about one to five minutes to effect complete relaxation.
  • Solutions of other swelling agents may be used as follows: potassium hydroxide 1.4%, lithium hydroxide 0.6%, sodium carbonate sodium sulfide 3.0% and potassium thiocyanate 3.0%
  • the accompanying drawing is a fiow sheet illustrating a typical operation carried out for the production of staple fibers according to the invention. It is to be understood that in the production of continuous filaments the cutting operation is to be omitted.
  • Example I A viscose of 7.5% cellulose and 6.5% sodium hydroxide content was prepared from Cordenier-J wood pulp containing 96.6 alpha cellulose, having an intrinsic viscosity of 6.0, degree of polymerization of 1140, and General Electric brightness of 89.
  • the viscose modified by addition at the mixing stage of 0.1% (based on the Weight of the viscose) dimethylamine and 0.1% polyethylene glycol (M.W. 1540), was extruded at 10.0 sodium chloride index through an 1100-hole spinnere'tte into a spin bath comprising 7.8% sulfuric acid, 16% sodium sulfate and 6.0% zinc sulfate.
  • the filaments were led through a bath-fed tube for 26 inches, combined with other lIOO-filament yarn ends and with strong primary bath still clinging thereto given a 5-stage progressive primary stretch of 100% with tension build-up to about one gram/denier maximum while still in an incompletely regenerated, plastic state.
  • the filaments were then led into a dilute, 4% sulfuric acid bath at 90 C. to impart a secondary stretch of an additional 30% at a tension of about one g./denier and to fix by completing regeneration.
  • the regenerated filaments were led onto a thread advancing drum showered with hot water to provide a preliminary wash, and then under a low tension of about 0.1 g./ denier wound up at 90 meters/minut on a cone with zero twist.
  • Cones of this yarn were pulled as a tow into a staple cutter to convert the tow into 1 /2 inch length staple, flowed down a stepwise chute with water to open, collected on a screen for washing and finishing.
  • the out staple of 1 /2 inch length and 1 /2 denier per filament was placed in a wire basket, washed by displacement through the mat to remove acid.
  • the mat of staple was then given a complete relaxation by displacement flow-through of 1% sodium hydroxide solution at 90 C. for one minute, then rewashed.
  • A. finishing wash was then given in water containing 0.1% S0 then centrifuged from an oil/water emulsion to leave 0.2% of a controlled friction finish in the staple (Nopco RSF #18).
  • the staple was then dried in a hot air steam.
  • Single filaments of this staple tested 4.0 grams per denier conditioned at 60% RH. and 75 F, 3.0 grams per denier wet and had an elongation of 22.0% when conditioned by subjecting them to 60% relative humidity at for a sufiicient time to bring the filaments to equilibrium. It was carded and spun into 30s and 40s count yarn, then woven into a fabric with ends/inch, and 80 picks/inch. The fabric was singed, desized, scoured and mildly bleached in conventional operations.
  • This fabric was subjected to a 50-cycle laundering evaluation alongside controls of similar construction fabric made from cotton, regular rayon, commercial high strength tire yarn-type rayon, high wet-modulus rayon, etc.
  • Example I An economical viscose composition containing 9.6% cellulose and 5.0% sodium hydroxide was prepared from Rayofiber-G wood pulp cellulose containing 96% alpha cellulose, having a cuene intrinsic viscosity 3.8, degree of polymerization of 750 and General Electric instrument brightness of 93. The viscose was modified by addition of the regeneration retardants, spun under staple conditions, given multi-stage primary stretch prior to regenerative fixing, converted into staple, and given relaxation in the manner outlined in Example I.
  • the finished single filament strengths were 3.8 grams per denier conditioned as in Example I, and 2.8 grams per denier wet with 21.0% elongation.
  • the color of the filaments was somewhat whiter than the filaments made in Example l, due to the pulp properties, and had enhanced dyeing characteristics of faster exhaustion and deep shade development.
  • the launderability of the fabric of this invention was outstanding, with shrinkage of less than 1% compared with 2% for cotton, 8% for regular rayon and 4% for the high wet-modulus rayon. Wear characteristics, as shown by accelerated laboratory tests and actual extended use were very good for this rayon, much superior to either the regular or high wet-modulus rayons.
  • Example IV The 80 x 80 fabric of Example I was singed, desized and dried. This fabric was then padded with a solution containing 4% of methylated melamine resin with 15% MgCl .6H O catalyst (based on resin Weight) and 0.2%
  • Example V Staple fiber of Example I was converted into 20s twoply yarn and knitted in mens socks using a 160-needle set-up. Following scouring and dyeing the socks were looped and boarded. These socks along with comparable socks made from cotton, regular rayon, several commercial improved rayons and high wet-modulus rayon were subjected to laundering and actual wear tests over a period of several weeks.
  • the socks from staple fiber of this invention invariably performed in a very superior manner compared with any of the other rayons, and were more or less equivalent to the cotton socks in all regards including both size stability and wear.
  • the improvement in the viscose process which comprises spinning viscose in an acid regenerating spin bath and stretching the filaments at least 90% in a primary stage while in contact with spin bath, then contacting the filaments which were not completely regenerated in the primary stage with a hot acid bath containing from 1% to 6% of sulfuric acid while stretching the filaments an additional 5% to 50% to completely fix and regenerate the filaments. prior to any relaxation and then subsequently immersing the filaments in an aqueous solution containing a swelling agent at an elevated temperature while the filaments are free to shrink to effect complete relaxation of the filaments producing washable filaments having practically no shrinkage and which can be converted into yarns and woven fabrics which exhibit dimensional stability during repeated severe laundering.
  • the swelling agent is a compound of the group consisting of sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium carbonate, sodium sulfide and potassium thiocyanate in aqueous solution in amounts of about 1%, 1.4%, 0.6%, 10%, 3% and 3% respectively.
  • the improvement in the viscose process which comprises spinning the viscose in a hot acid spin bath and stretching the filaments at least 90% while in contact with the spin bath or spin bath carryover to produce filaments containing an appreciable portion of skin, then contacting the filaments with a solution containing about 4% of sulfuric acid while stretching the filaments an additional 20% to eliminate the residual xan'thate and effect complete regeneration, washing the filaments, and then contacting the filaments at zero tension while free to shrink with an aqueous swelling solution containing an alkali metal hydroxide at about 90 C. to eflect complete relaxation.

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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)
US78779A 1960-12-27 1960-12-27 Viscose process for the manufacture of low-shrink rayon Expired - Lifetime US3046082A (en)

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NL272684D NL272684A (en(2012)) 1960-12-27
US78779A US3046082A (en) 1960-12-27 1960-12-27 Viscose process for the manufacture of low-shrink rayon

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3163185A (en) * 1962-09-28 1964-12-29 Kendall & Co Dimensionally stable, directionally stiff woven fabric
US3364290A (en) * 1962-10-30 1968-01-16 American Enka Corp High tenacity rayon yarn production
US20150252500A1 (en) * 2012-09-24 2015-09-10 Glanzstoff Bohemia S.R.O. Yarn having flame-retardant effect and textile fabric formed therefrom
US11529513B2 (en) 2013-11-27 2022-12-20 Ebt Medical, Inc. Neuromodulation system

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2491938A (en) * 1944-10-18 1949-12-20 Rayonier Inc Method of producing viscose filaments
US2611928A (en) * 1948-11-23 1952-09-30 American Viscose Corp Method for producing high tenacity artificial yarn and cord
US2952508A (en) * 1953-09-16 1960-09-13 Rayonier Inc Viscose process and products produced thereby

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2491938A (en) * 1944-10-18 1949-12-20 Rayonier Inc Method of producing viscose filaments
US2611928A (en) * 1948-11-23 1952-09-30 American Viscose Corp Method for producing high tenacity artificial yarn and cord
US2952508A (en) * 1953-09-16 1960-09-13 Rayonier Inc Viscose process and products produced thereby

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3163185A (en) * 1962-09-28 1964-12-29 Kendall & Co Dimensionally stable, directionally stiff woven fabric
US3364290A (en) * 1962-10-30 1968-01-16 American Enka Corp High tenacity rayon yarn production
US20150252500A1 (en) * 2012-09-24 2015-09-10 Glanzstoff Bohemia S.R.O. Yarn having flame-retardant effect and textile fabric formed therefrom
US11529513B2 (en) 2013-11-27 2022-12-20 Ebt Medical, Inc. Neuromodulation system

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