Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K5/00—Use of organic ingredients
  • C08K5/04—Oxygen-containing compounds
  • C08K5/07—Aldehydes; Ketones
• • 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
• • 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 generally to the manufacture of rayon threads, fibers, yarn and the like products hereinafter referred to collectively as yarn and more particularly to the production of high modulus viscose rayon yarn characterized by its high strength and low elongation values making it especially suitable for use in rug backing and in reinforcing rubber products such as belting and the like.
• Yarn having high strength and low elongation values is commonly referred to as high modulus yarn.
• the modulus of yarn is determined by the following formula:
• M modulus
• S break strength in grams per denier
• E percent of elongation
• a process of particular significance is that disclosed in application Serial No. 740,189, having common ownership herewith, wherein a viscose containing an ethoxylated amine modifier is extruded into an acid spinning bath.
• the threads thus-produced are then aftertreated by passing them through a cold intermediate bath con taining formaldehyde, and then through a hot stretch bath.
• a cold intermediate bath con taining formaldehyde and then through a hot stretch bath.
• Patent N01 3,007,766 a viscose containing an alkali metal salt and modifiers, such as polyethylene glycol, ethoxylated amines and their quaternized derivatives is extruded into an acid spinning bath followed by passing the thus-produced threads through an intermediate bath containing formaldehyde and then through a hot acid stretch bath also containing formaldehyde.
• an alkali metal salt and modifiers such as polyethylene glycol, ethoxylated amines and their quaternized derivatives
• An additional object of this invention is to provide a simple and economical process for producing high modulus viscose rayon yarn.
• Another object is to provide a process for producing high modulus viscose rayon yarn having high strength and low elongation values.
• a still further object of this invention is. to provide a process for producing viscose rayon yarn utilizing a novel combination of modifiers whereby a viscose rayon yarn with improved physical properties is produced;
• the amount of formaldehyde used may vary within a range of from 0.05% to 1.0%, based on oven dry recoverable cellulose in viscose (hereinafter abbreviated as The preferred amount of formaldehyde is 0.5% CiV. While amounts higher than 1.0% CiV may be used, such increased amounts result in no further improvement in the yarn.
• the formaldehye is used in combination with other so-called modifiers in the viscose such as the polyglycols, alkoxylated amines, and their quaternary derivatives.
• the alkoxylated amines are known in the art as Ethomeens and are described in detail in US. Patent No. 2,978,292, the disclosure of which is incorporated herein by reference.
• Their quaternary derivatives are known as Ethoquads and are described in detail in application Serial No. 609,792, filed September 14, 1956, having common ownership herewith.
• the polyglycol used is preferably either polyethylene glycol or polypropylene glycol, the molecular weight of which may vary depending upon the spinning conditions and the particular amine employed. These modifiers may be present to the extent of 0.3% to 5.0% CiV.
• the source of the cellulose may be wood pulp, cotton linters, or a mixture thereof.
• the cellulose content of the viscose may range from about 5.0%-8.5%.
• the amount of carbon disulfide used during the xanthation *Registered trademarks of Armour and Company.
• step may vary from 25-60% CiV, with the preferred amount being 38%-40%.
• the viscose is aged to approximately the same level of maturity before spinning as that normally used.
• a 7.3-5.5 (percent cellulose-percent total alkali) viscose may have a Hottenroth maturity index varying at spinning from about 8-20.
• Viscose prepared in accordance with this invention is extruded into an acid primary bath, from which the filaments thus-produced are withdrawn and highly stretched, preferably in a hot acidic secondary bath. They are then aftertreated in the usual manner.
• the primary spinbath contains an aqueous solution of from 2%-10% sulfuric acid, 3%-26% sodium sulfate and 1%-9% zinc sulfate.
• other metal salts may be substituted for the zinc sulfate.
• the total salt content should not exceed 15%.
• modifiers such as the alkoxylated amines may be present in small quantities. Stretching is preferably carried out in a dilute sulfuric acid containing second bath, maintained at a temperature of about 80100 C. Small quantities of sodium and Zinc sulfates may also be present in this bath. The spinning stretch is preferably adjusted to 1 gram per denier.
• Example I Alkali cellulose was prepared in the conventional manner from wood pulp and aged to obtain a degree of polymerization that would yield a viscose solution viscosity of 50-60 seconds by the ball fall method.
• a viscose was obtained having a composition of 7.3% cellulose, 5.5% sodium hydroxide and 2.25% total sulfur.
• the freshly prepared viscose solution was deaerated, filtered, and ripened to a Hottenroth maturity index of about 13.5.
• the viscose solution was extruded into a primary spinbath containing 5.0% H 8.5% Na SO 5.0% ZnSO plus 1000-2000 parts per million of Ethomeen C-25.
• the temperature of the spinbath was maintained at 42 C.
• the yarn was withdrawn and passed through a secondary bath containing 3.0% H 80 1.4% Na SO and 0.5% ZnSO maintained at a temperature of 92 C. for an immersion distance of 40 inches.
• the yarn thus produced was then collected in a rotating pot.
• a tension of 1600 grams was maintained in the secondary bath to produce a stretch of
• the collected yarn was aftertrealted in the conventional manner and tested for strength and elongation in both conditioned and wet state.
• the properties of the yarn are set forth in Table II.
• Example II Five 73/ 5.5/ 2.3 (percent cellulose-percent total alkalipercent total sulfur) viscoses were prepared in a manner similar to that described in Example I. One was a contnol and contained no formaldehyde. The other four contained varying amounts of modifiers. All were aged to a Hottenroth maturity index of 16-20. Samples of each were extruded into spinbaths containing different percentages of H 80 The other additives to the spinbath were held constant at 8.5% Na SO and 5.0% ZnSO The primary spinbaths were maintained at a temperature of 42 C. with the immersion distance being 28 inches. The secondary baths all contained 2.4% H 50 1.1% Na SO and 0.5 ZnSO and were maintained at 92 C. Tension was adjusted to 1100 grams per denier. All yarn samples contained 1100 filaments and averaged approximately 1100 denier.
• Example III Five 73/55/225 (percent cellulose-percent total alkali-percent total sulfur) viscoses were prepared using the same procedure as that described in Example I. All were aged to a Hottenroth maturity index of 1314.5. Viscosity was 5060 seconds, ball fall method. Diifen ent percentages of formaldehyde were used in each sample, the remaining additives being constant at 0.5% CiV polyethylene glycol and 2.0% CiV Ethomeen C-25. Each viscose was extruded into a spinbath containing 5.0% H 80 8.5% Na SO and 5.0% ZnSO plus 1000-2000 parts per million Ethorneen C-25. Temperature of the spinbath was maintained at 42 C., with immersion for 24 inches. The secondary bath composition was 3.0% H SO 1.4% Na SO and 0.5% ZnSO With the temperature being 93 C. Immersion distance was 40 inches. Tension and stretch were the same as in Example I. The
• a high strength low elongation and high modulus yarn can be prepared in accordance with this invention by incorporating formaldehyde in the viscose.
• Such procedure eliminates the use of an expensive intermediate bath system. Most important, however, escaping formaldehyde fumes, necessarily present with the intermediate bath system are likewise eliminated.
• elongation viscose rayon yarn and like products which comprises extruding a viscose solution containing from 0.05% to 0.5 formaldehyde, based on the cellulose in viscose, prepared by adding the formaldehyde to the dissolving lye for the cellulose xanthate, and from 0.3% to 5.0% of a modifier based on the cellulose in the viscose, said modifier selected from the group consisting of polyglycols, alkoxylated amines, and their quaternized derivatives, into an acid coagulating and regenerating bath, and collecting the yarn.
• the improvement comprising dissolving the cellulose xanthate crumbs in a caustic soda solution containing from 0.05% to 1.0% formaldehyde based on the cellulose in viscose and from 0.3% to 5.0% of a modifier based on the cellulose in viscose, said modifier selected from the group consisting of polyglycols, alkoxylated amines, and their quaternized derivatives, spinning the viscose into an acid coagulating and regenerating bath and stretching the resultant filaments whereby a high strength, low elongation filamentary product is obtained.
• the improvement comprising dissolving the cellulose xanthate crumbs in a caustic soda solution containing from 0.05% to 1.0% formaldehyde based on the cellulose in viscose, incorporating from 0.3% to 5.0% of a modifier based on the cellulose in viscose in the resultant viscose solution prior to spinning, and modifier selected from the group consisting of polyglycols, allcoxylated amines, and their quaternized derivatives, spinning the viscose into an acid coagulating and regenerating bath, and stretching the resultant filaments whereby a high strength, low elongation filamentary product is obtained.
• a process for producing high strength, low elongation rayon products comprising dissolving cellulose Xanthate crumbs in a caustic soda solution containing from 0.05% to 1% formaldehyde based on the cellulose in viscose and from 0.3% to 5% of a modifier based on the cellulose in viscose, said modifier selected from the group consisting of polyglycols, alkoxylated amines, and their quaternized derivatives, aging the resultant viscose solution, spinning the aged viscose into an acid and coagulating and regenerating bath and thereafter stretching the thus produced product.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Health & Medical Sciences (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Artificial Filaments (AREA)

Priority Applications (9)

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Publications (1)

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Cited By (1)

Citations (2)

• 0
  • NL NL287417D patent/NL287417A/xx unknown
  • BE BE626103D patent/BE626103A/xx unknown
• 1962
  • 1962-01-17 US US166908A patent/US3153687A/en not_active Expired - Lifetime
• 1963
  • 1963-01-04 CH CH8463A patent/CH410270A/de unknown
  • 1963-01-11 DE DEA42064A patent/DE1220081B/de active Pending
  • 1963-01-14 GB GB1612/63A patent/GB962622A/en not_active Expired
  • 1963-01-16 AT AT33663A patent/AT243427B/de active
  • 1963-01-16 ES ES284208A patent/ES284208A1/es not_active Expired

Patent Citations (2)

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