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EP0049710A1 - Kräuselfasern aus regenerierter Zellulose, Verfahren zu deren Herstellung und diese Fasern enthaltende Gewebe - Google Patents

Kräuselfasern aus regenerierter Zellulose, Verfahren zu deren Herstellung und diese Fasern enthaltende Gewebe Download PDF

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Publication number
EP0049710A1
EP0049710A1 EP80106223A EP80106223A EP0049710A1 EP 0049710 A1 EP0049710 A1 EP 0049710A1 EP 80106223 A EP80106223 A EP 80106223A EP 80106223 A EP80106223 A EP 80106223A EP 0049710 A1 EP0049710 A1 EP 0049710A1
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EP
European Patent Office
Prior art keywords
viscose
bath
cellulose
sulfuric acid
filaments
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Granted
Application number
EP80106223A
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English (en)
French (fr)
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EP0049710B1 (de
Inventor
Gregory Christopher Bockno
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Akzo Nobel UK PLC
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Avtex Fibers Inc
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Priority to DE8080106223T priority Critical patent/DE3071017D1/de
Priority to AT80106223T priority patent/ATE15082T1/de
Priority to EP80106223A priority patent/EP0049710B1/de
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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
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/01—Natural vegetable fibres
    • D10B2201/02—Cotton
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/20—Cellulose-derived artificial fibres
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/20—Cellulose-derived artificial fibres
    • D10B2201/22—Cellulose-derived artificial fibres made from cellulose solutions
    • D10B2201/24—Viscose
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/06—Load-responsive characteristics
    • D10B2401/063—Load-responsive characteristics high strength

Definitions

  • This invention relates to the production of regenerated cellulose or viscose rayon fibers and filaments. More specifically the invention is directed to the production of crimped, high-wet modulus type viscose rayon fibers and filaments
  • viscose rayon fibers and filaments have had a wide acceptance.
  • Low-wet modulus viscose rayon fibers typically referred to commercially as regular rayon are characterized in fabric form by excessive shrinkage when wet and then dried, and by a relatively low modulus in the wet state. Such fibers have a wet modulus of about 2.5 to 3.0 gm./denier.
  • the use of high wet modulus fibers in fabric has demonstrated their utility in terms of improved fabric yield and in overall fabric performance as it relates to consumer use.
  • Such fibers have a wet modulus of 5 to 15 gm./denier and this range encompasses typical wet modulus values for most cottons.
  • modifying agents in the viscose, particularly polyalkylene glycols, ethoxylated fatty acids, fatty alcohols or fatty esters and ethoxylated higher aliphatic amines.
  • the use of the modifying agents has resulted in increases in the tenacity and abrasion resistance of the fibers and filaments.
  • the present invention provides a method of producing crimped high-wet modulus rayon fibers which are characterized generally by high strength, high wet modulus, a low water pickup and low shrinkage in fabric form but without the use of viscose modifiers.
  • the invention also provides viscose rayon fibers having high wet and conditioned moduli and high wet and conditioned strengths.
  • This invention further provides a more economical method of producing high wet modulus viscose rayon fibers and filaments. It also reduces BOD loading in waste treatment from the wash water of the process.
  • the present invention contemplates the production of crimped, high strength, high wet modulus viscose rayon fibers by utilizing modifier-free viscose and spinning baths having compositions within selected limits and spinning the viscose under a limited range of conditions.
  • the method is applicable to the production of staple fibers in a wide range of deniers in accordance with conventional practice.
  • the viscose solution is converted into a plurality of filaments or tow which is cut to the desired fiber length to produce rayon staple.
  • fiber will be used in the specification and it is to be understood that the term also refers to staple fibers.
  • the fibers of this invention may be used as a replacement for cotton in many textile constructions. They also may be blended with cotton. These fibers retain the usual desirable characteristics of rayon fibers, such as processability, dyeability, fabric finishing, and moisture regain. Both bright and delustered fibers can be made. Fabrics produced from these fibers are firm and cotton-like with respect to hand. This enhancement of fabric hand results from the unique combination of fiber cross-sectional shape and fiber modulus.
  • Fibers of this invention may be advantageously employed in blends with cotton, polyester, acrylic, or other synthetic fibers wherein the rayon content may be from 1 to 99%.
  • the wet modulus expressed as grams per denief, as used herein is an average initial wet modulus which is defined as wet modulus
  • the wet modulus is a measure of the resistance of the wet fiber to stretching when subjected to tension.
  • Reported values of percentage elongation represent the amount of stretching in a fiber placed under tension as percentage of original fiber length at the break point.
  • Measurements of wet modulus and % elongation of single fibers may be made on an Instron Tensile Tester.
  • the wet modulus of the viscose rayon fiber of the present invention varies between about 5.0 and 12 g/d, whereas low wet modulus rayon has a wet modulus of about 2.5 to 3 g/d.
  • the % elongation of this fiber is generally within the range of from 14% to 27% when wet, and about 11% to 22% in the conditioned state.
  • the breaking tenacity (hereafter'tenacity) of the fiber is generally within the range of from 1.5 to 2.7 grams per denier when wet, and about 2.R to 4.0 grams per denier in the conditioned state.
  • the high wet modulus fibers produced in accordance with Patent No. 4,121,012 have highly desirable physical properties and characteristics.
  • fibers-produced in accordance with that patent are characterized in having a substantially ovate section with from about 25 to 30% skin.
  • fibers made in accordance with the present invention do not require the use of modifying agents, thus eliminating costs associated with use of such agents and the attendant pollution problem.
  • the present fibers have, in contrast, a highly desirable unsymmetrical, multilobular, skin-core type cross-section which provides a distinct improvement in fabric cover and a distinctly firmer (crisper) hand.
  • the skin which is interrupted or discontinuous as illustrated in Fig. 3, constitutes from about 20% to about 35% of the cross-section.
  • the fibers have from 10 to 30 crimps per inch (cpi).
  • the fibers and filaments of the present invention are obtained by proper adjustment of the interrelated parameters of the viscose process, namely the viscose composition, the metnod of preparation, the spinning bath composition, and the spinning conditions.
  • the viscose contains from 6% to 10% cellulose and from 4% to 9% caustic soda.
  • the cellulose xanthate of the viscose is prepared by addition of from about 28% to 45% (preferably 30% to 32%) carbon disulfide, based upon the weight of the cellulose to the alkali cellulose.
  • Alkali cellulose is prepared by steeping commercially available high quality dissolving grade wood pulp in steeping presses or in continuous steeping equipment using aqueous solution of caustic soda for up to about one hour at ambient temperatures.
  • the alkali cellulose is pressed to a press weight ratio of about 2.8 to 2.9 : 1.
  • the pressed alkali cellulose is shredded and mercerized in the usual manner. It is then xanthated by the addition of the major proportion of carbon disulfide.
  • the resulting xanthated alkali cellulose is dissolved in a caustic soda solution and the balance of the carbon disulfide added during the dissolving step.
  • the step-wise addition of carbon disulfide commonly referred to as split xanthation is not essential, it is merely an alternate procedure for accomplishing the degree of xanthation desired.
  • the viscose is ripened at a temperature between about 9°C. and 22°C. for up to about 30 hours (including the mixing and holding periods). Viscose formed as described will exhibit a salt test of from about 5.5 to 15 (preferably 6.0 to 8.5) and a spinning ball fall viscosity of 60 to 110 seconds.
  • the total sulfur content will vary from about 2.1 to about 3.4% and the xanthate sulfur will vary from about 1.4 to about 3.4%.
  • the spinning bath should contain between 4% and 8% sulfuric acid, 0.5 to 3% zinc sulfate and from 16% to 22% sodium sulfate.
  • the temperature of the bath should be maintained between about 40° and 65°C, preferably 40°C and 60°C, and the spinning speed, as measured at the tow roll, should be about 25 to 60 meters per minute which results in a calculated residence time of the tow in the spin bath of 0.66 to 7.5 seconds.
  • the filaments, prior to washing are passed through a second bath or stretch bath maintained at a temperature between about 80°C.
  • the filaments are stretched from about 65% to about 120% (preferably 73 - 100%) during the travel through this bath.
  • the residence time of the tow in the spin bath can be controlled to obtain the desired stretch specification.
  • the stretch bath may be a hot water bath, a very dilute solution of sulfuric acid, or it may be a diluted spinning bath containing from 0.5 to 4.0% sulfuric acid, 0.1 to 2.0 % zinc sulfate and 3 to 12% sodium sulfate.
  • the fibers produced are subsequently subjected to the normal after-treatments such as washing, desulfurizing and bleaching by well known methods.
  • Viscose was prepared by treatment of pulp sheets (98% alpha-cellulose, dissolving grade pulp,) with caustic soda, shredding the resulting alkali cellulose, xanthating the alkali cellulose and dissolving it in a caustic soda solution.
  • the viscose so prepared contained 7.5% cellulose, 7.5% caustic soda and 34% carbon disulfide, based on the weight of the cellulose.
  • the viscose at the time of spinning had a sodium chloride salt test of about 8.5, and a ball-fall viscosity of 70 to 80 seconds. Ball-fall viscosity is obtained by measuring the time in seconds required for a solid steel ball of 1/8 inch diameter . to fall 8 inches in a column of viscose of 3/4 inch diameter at - 18°C.
  • the dimethylamine and phenol ether modifiers may be added at any stage in the preparation of the viscose to serve as a regeneration retardant.
  • the viscose was spun to form a 1.5 dpf, 12,000 filament tow by extrusion of the viscose through orifices about 0.0025 inch in diameter into a spinning bath containing 5% sulfuric acid, 17% sodium sulfate and 3% zinc sulfate, the spinning bath being maintained at a temperature of about 48°C.
  • the filaments were withdrawn from the bath, passed over a first godet, through a hot second bath, over a second godet, cut into staple, sluiced, after- treated, and dried.
  • the second bath was formed by diluting some of the spinning bath and contained about 2.5% sulfuric acid, about 1.5% zinc sulfate and about 8% sodium sulfate, and was maintained at a temperature of about 95°C. During passage of the filaments through the hot bath, they were stretched approximately 115%. The spinning speed was about 25 meters per minute. The wet yarn was cut into staple length fibers and dropped into a water sluice bath maintained at about 90°C. The staple fibers formed from 25 to 30 crimps per inch in the sluice bath. The crimped staple was then wet processed and dried.
  • the crimped fiber had a conditioned tenacity of about 4 grams per denier, a wet tenacity of about 2.7 grams per denier, a conditioned extensibility of about 14 percent, a wet extensibility of about 19 percent, an initial wet modulus of about 10.0, and was a substantially non-fibrillatable fibrous product.
  • a representative filament had a smooth, broken skin which comprised about 25% of the cross-sectional area and encompassed about 65% of the periphery of the cross-section.
  • the core was "broken-out" of the filament cross-section to provide an unbalanced shape.
  • Viscose was prepared as described in Example 1 with the exception that 1% dimethylamine and 2% of the polyoxyethylene glycol ether of phenol were incorporated into the viscose.
  • the viscose had a sodium chloride salt test of 8.7 and a ball fall viscosity of 80 - 90 seconds.
  • the total sulfur content was about 1.9% and the xanthate sulfur was about 1.5%.
  • the viscose contained 7.5 % cellulose, and 7.5% caustic soda.
  • a total of 31% carbon disulfide based upon the weight of the cellulose was added during xanthation and dissolving.
  • the viscose was ripened at 18°C. to obtain at time of spinning a sodium chloride salt test of 8.0 to 9.0, and a ball fall viscosity of 75 seconds.
  • the viscose was spun to form a 12,000 filament tow by extrusion of the viscose through orifices 0.0025 in. in diameter.
  • the spinning bath contained 5.6 - 6.0% sulfuric acid, 2.6 - 2.7% zinc sulfate and 17.3 - 17.9% sodium sulfate and was maintained at a temperature of 48°C. After an immersion of 21 inches (53 cm.), the filaments were withdrawn from the bath, passed over a first godet to a cascade bath, the bath temperature being about 95°C., over a second godet, cut into staple lengths, sluiced in hot water (95°C.), after-treated and dried.
  • the second bath was formed by diluting the spinning bath and contained about 2.5% sulfuric acid, about 1.5% zinc sulfate and about 8% sodium sulfate. During passage of the filaments through the hot bath, they were stretched approximately 105%. The spinning speed was 30 meters per minute. The fibers when sluiced in hot water formed 21 - 25 crimps per inch (cpi). The fibers had a linear density of 1.5 denier.
  • a representative filament of the present invention was formed in accordance with the following example.
  • Alkali cellulose was prepared by steeping a 98% alpha cellulose rayon grade dissolving pulp in 19% aqueous caustic soda, and pressing the steeped sheets to a press weight ratio of 2.8 to 1, followed by shredding and mercerizing the resulting alkalli cellulose.
  • Two-stage xanthation was effected by introducing about 85 % of the carbon disulfide to the alkali cellulose in the xanthator and the balance of the carbon disulfide was added to the mixer during dissolving of the xanthate in the caustic soda solution.
  • the viscose thus prepared contained 7.5% cellulose, and 7.5% caustic. soda.
  • a total of 31% carbon disulfide based upon the weight of the cellulose was added during xanthation and dissolving.
  • the viscose was ripened at 10°C. for about 22 hours. At the time of spinning, the viscose had a sodium chloride salt test of 8.4 and a ball fall viscosity of 67 seconds.
  • the total sulfur content was 1.96% and the xanthate sulfur was 1.49%.
  • the viscose was spun to form a 12,000 filament tow by extrusion through orifices about 0.0025 in. in diameter into a spinning bath containing 6.1% sulfuric acid, 2.6% zinc sulfate and 20.9% sodium sulfate, the bath being at a temperature of about 48°C.
  • the filaments after 21 in. (53 cm.) immersion were withdrawn from the bath, wrapped over a godet, then passed through a hot second bath, wrapped over a second godet, and collected.
  • the tow was then cut into staple lengths, sluiced in hot water (95°C.) during which fiber crimp developed, aftertreated and dried.
  • the second bath was formed by diluting some of the spinning bath and contained about 2.5% sulfuric acid, about 1.5% zinc sulfate and about 8% sodium sulfate and was maintained at temperature of 95°C.
  • the filaments were stretched approximately 99%.
  • the spinning speed was 30 meters per minute.
  • the filaments were cut into staple lengths and then sluiced in hot water forming 22 - 25 crimps per inch (cpi).
  • the staple fibers were purified by washing, desulfurizing, finishing with a lubricant, and dried by usual methods. Linear density of the fiber was 1.5 denier.
  • the average degree of polymerization (D.P.) of these cellulose fibers is 485 (range of 450 - 525).
  • Fibers of this embodiment preferably have a wet tenacity of between 2.0 and 2.3, a conditioned tenacity of between 3.6 and 3.8 grams per denier, a wet % elongation between 25 and 27%, a conditioned % elongation between 17 and 20%, and a wet modulus between 6.0 and 7.0.
  • the Wet Stiffness Factor as reported in Table I is the wet strength in grams per denier divided by the percent elongation in the wet state.
  • Example 3 includes preferred viscose and spinning bath compositions and spinning conditions.
  • the fibers formed as described are representative of fibers formed within the range set forth hereinbefore. This is demonstrated by the data in Table IV that summarizes compositions and conditions - within the stated ranges.
  • the viscoses were prepared as described in Example 3 and had the compositions as set forth in Table IV.
  • Each viscose was spun into the stated spinning bath to form a 12,000 filament tow at a spinning speed of 30 meters per minute.
  • the fibers had a linear density of 1.5.
  • the stretch baths had approximately the same composition and were at the same temperature as that used in Example 3.
  • Example 3 is included in Table II for purposes of comparison.
  • Fabrics formed of fibers of the present invention exhibit significantly enhanced fabric hand, being firm and lacking the limpness of rayon fabrics. The hand is similar to-that of cotton, but this is not true of the fabrics made from fibers of Examples 1 and 2.
  • Fabric formed of fibers of the present invention also exhibit a distinct improvement in cover, as judged by this opacity which is visually readily observable and is further confirmed by light transmittance inastandardized test conducted on an Ozalid printer. These improvements in hand and cover are imparted by a combination of the multilobal cross-section, the fiber crimp, and the higher modulus. These physical attributes lead to a low packing factor in yarns prepared from the fibers.
  • Table I illustrates that the filaments and fibers prepared in accordance with the present invention have attractive tensile properties, although not identical to filaments and fibers prepared in accordance with the methods disclosed in U. S. Patent No. 3,277,226 and U. S. Patent No. 4,121,012.
  • the most distinctive difference between the products characterized in Table 1 is, that while the fibers prepared in accordance with the U. S. Patent No. 3,277,226 (substantially circular in cross-section as shown by Figure 1), and U. S. Patent No. 4,121,012 (ovate in cross-section as shown in Figure 2), the fibers of the present invention have a highly desirable, unsymmetrical, multilobular cross-section, as illustrated by Figure 3.
  • the present invention may also be represented by a fiber formed in an alternate embodiment in accordance with the following example.
  • Alkali cellulose was prepared by steeping a 93% alpha cellulose rayon grade dissolving pulp in an 18% caustic soda solution and pressing to a press weight ratio of 2.8tol. By the.usual techniques of steeping, a hemi-rich fraction of caustic soda was obtained and was reserved for use in viscose mixing.
  • the resulting alkali cellulose was shredded and mercerized at 18°C. for 18 hours.
  • Xanthation was accomplished by one step addition of carbon disulfide.
  • Virgin caustic soda mixed with hemi-rich reject soda and water was used to dissolve the xanthated crumb.
  • the viscose thus prepared contained 9.2% cellulose and 6.0 caustic soda. It was prepared by the addition of 30% carbon disulfide, based upon the weight of the cellulose.
  • the viscose was ripened at 18.5°C. for about 21 hours. At the time of spinning the viscose had a sodium chloride salt index of 6.0 and an average ball fall viscosity of 70 seconds.
  • the total sulfur content was 2.3% and the xanthate sulfur was 1.4%.
  • the viscose was spun tr form 12,000 filament tow by extrusion through orifices of 0.0025 in. in diameter into a spinning bath containing 5.7% sulfuric acid, 0.9% zinc sulfate, and 20 % sodium sulfate, the bath being at a temperature of 60°C.
  • the filaments were withdrawn from the bath, after a tow immersion of 24 inches, and wrapped on a godet and then passed through a hot regeneration bath, wrapped on a tow roll, collected and after- treated.
  • the hot regeneration bath was prepared by diluting some of the spinning bath and contained 2.5% sulfuric acid, about 0.4 % zinc sulfate and about 8.0% sodium sulfate and maintained at a temperature of 93°C.
  • Fibers of this embodiment have a wet tenacity between 1.7 and 1.8 grams per denier, a conditioned tenacity between 3.2 and 3.3 grams per denier, a wet % elongation between 15 and 18%, a conditioned % elongation between 12 and 14%, a wet modulus between 8.0 and 10.0, and 10 to 12 crimps per inch.
  • Another embodiment of the present invention was formed in accordance with the following example.
  • Alkali cellulose was prepared by steeping 96% alpha cellulose, rayon grade dissolving pulp, in an 18% caustic soda solution and pressing to a press weight ratio of 2.85 to 1. By the usual techniques of steeping, a hemi-rich fraction of caustic soda was obtained and was reserved for use in viscose mixing.
  • the resulting alkali cellulose was shredded and mercerized at 18°C. for 20 hours.
  • Xanthation was accomplished by one step addition of carbon disulfide.
  • Virgin caustic soda mixed with hemi-rich reject soda and water was used to dissolve the xanthated crumb.
  • the viscose had a composition of 7.5 % cellulose, 7.5% caustic soda. It was prepared by the addition of 32.5% carbon disulfide (based on weight of cellulose).
  • the viscose was ripened at 23°C. for about 20 hours. At the time of spinning, the viscose had a sodium chloride salt test of 8.2 and a ball fall of 76 seconds. The total sulfur content was 1.99% and the xanthate sulfur was 1.50%.
  • the viscose was spun to form a 28,500 filament tow by extrusion through orifices having 0.0020 diameter in a spinning bath containing 5.9% sulfuric acid, 21.4% zinc sulfate, and 18.2% sodium sulfate, the bath being at a temperature of about 47° C.
  • the filaments after 23 inches (58 cm) immersion were withdrawn from the bath wrapped over a godet, then passed through a hot reneneration bath and finally wrapped on a tow roll.
  • the regeneration was formed by diluting some of the spin bath and contained 2.2% sulfuric acid, 0.85% zinc sulfate, and 6.6% sodium sulfate and was maintained at a temperature of 90 - 92° C.
  • the tow filaments were stretched 92% between the godet and the tow roll with the tow roll delivering stretched tow at 29.3 meters per minute.
  • the tow was then fed to a cutter to produce staple fibers which were washed, desulfurized, and finished with a lubricant.
  • the staple was then dried by commercial rayon manufacturing methods.
  • Alkali cellulose was prepared by steeping 96% alpha Cellulose, rayon grade dissolving pulp, in an 19% caustic soda solution and pressing to a press weight ratio of 2.80 to 1. By the usual techniques of steeping, a hemi-rich fraction of caustic soda was obtained and was reserved for use in viscose mixing.
  • the resulting alkali cellulose was shredded at 33° C . and mercerized at 31° C. for 18 hours.
  • Xanthation was accomplished by one step addition of carbon disulfide. Virgin caustic soda mixed with hemi-rich reject soda and water was used to dissolve the xanthated crumb. After final mixing, the viscose had a composition of 7.55 % caustic soda. It was prepared by the addition of 30% carbon disulfide (based on weight of cellulose).
  • the viscose was ripened at an average of 20°C. for about 26 hours. At the time of spinning, the viscose had a sodium chloride salt test of 5 .7 and a ball fall of 85 seconds. The total sulfur content was 1.85% and the xanthate sulfur was 1.38%.
  • the viscose was spun to form a 28,500 filament tow by extrusion through orifices having 0.0020 inch diameter in a spinning bath containing 5.5% sulfuric acid, 2.85% zinc sulfate, and 16.5% sodium sulfate, the bath being at a temperature of about 41°C.
  • the filaments after 21 inches (53 cm) immersion were withdrawn from the bath, wrapped over a godet, then passed through a hot regeneration bath and finally wrapped on a tow roll.
  • the regeneration bath was formed by diluting some of the spin bath and contained 2.5% sulfuric acid, 0.90% zinc sulfate, and 8.0% sodium sulfate and was maintained at a temperature of 90 - 92°C.
  • the tow filaments were stretched an average 92% between the godet and the tow roll with the tow roll delivering streth- ed tow at 29.3 meters per minute.
  • the tow was then fed to a cutter to produce staple fibers which were washed, desulfurized, and finished with a lubricant.
  • the staple was then dried by commercial rayon manufacturing methods.
  • the present invention provides regenerated cellulose fibers having a wet tenacity of at least about 1.5 grams per denier, in general varying. up to about 2.7 grams per denier.
  • the fibers In the conditioned state, that is, after the fibers have been initially dried and then held in an atmosphere having a temperature of 75°F. (24°C) and a relative humidity of 58% for twenty-four hours, the fibers have a tenacity of between about 2.8 and 4.0 grams per denier.
  • the fibers have a wet modulus of between 5.0 and 12, a wet % elongation of between about 14% and 26% and a conditioned % elongation of between about 11% and 22%.
  • the fibers are further characterized in having a skin-core structure, wherein the core is surrounded by a discontinuous, broken skin and being multilobular in cross-section.
  • the method of the present invention includes the use of a modifier-free viscose containing from 6% to 10% cellulose, from 4% to 9% caustic soda and from 28% to 45% carbon disulfide, based on the weight of the cellulose, ripened at a temperature of from 9°C. to 22°C. for up to about 30 hours and having a salt test of from about 5.5 to 15, such as, for example, 7.5% cellulose, ripened at 18°C. for 22 hours and having a salt test of 8.0 to 8.5.
  • a modifier-free viscose containing from 6% to 10% cellulose, from 4% to 9% caustic soda and from 28% to 45% carbon disulfide, based on the weight of the cellulose, ripened at a temperature of from 9°C. to 22°C. for up to about 30 hours and having a salt test of from about 5.5 to 15, such as, for example, 7.5% cellulose, ripened at 18°C. for 22 hours and having a salt test of
  • the viscose is spun at a spinning speed of 20 to 60 meters per minute into a spinning bath containing 4% to 8% sulfuric acid, 0.5% to 3.0% zinc sulfate and 17% to 22% sodium sulfate maintained at a temperature of between 40°C. and 65°C., such as, for example, 6.2% sulfuric acid, 2.5% zinc sulfate and 17.5% sodium sulfate maintained at about 48°C.
  • the filaments are stretched from about 65% to 120% in a hot, dilute acid bath, 88°C. to 95°C., consisting of from 1% to 4% sulfuric acid, from .3% to 12% sodium sulfate, and from 0.3% to 1.2% zinc sulfate, e.g. 3.4% H 2 S0 4 , 1.75% ZnSO and 5.4% Na 2 So 4 at a temperature of 90°C.
  • the present method results in a reduction in the fiber manufacturing cost, by eliminating the need for viscose modifiers typically used for producing HWM fibers.
  • the elimination of these viscose modifiers reduces costs with respect to the cost of the modifiers and of reducing BOC loading of plant effluent waste waters.
  • the economic advantages are achieved in addition to obtaining the essential and desirable fibers properties, and the consequent desirable improvement in fabrics achievable with the fibers of this invention.
  • a crimp measurement for staple fibers is made by removing small bundles of fibers (approximately 10 fibers) from where the crimp of the fibers appears to be in phase. The fiber are laid on a black felt in a linear relationship. The number of crimps are counted over a one inch lineal dimension without extending the fibers in the linear dimension, wherein a crimp is designated as a change in direction of the fibers.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
EP80106223A 1980-10-13 1980-10-13 Kräuselfasern aus regenerierter Zellulose, Verfahren zu deren Herstellung und diese Fasern enthaltende Gewebe Expired EP0049710B1 (de)

Priority Applications (3)

Application Number Priority Date Filing Date Title
DE8080106223T DE3071017D1 (en) 1980-10-13 1980-10-13 Crimped regenerated cellulose fibers, a method for their preparation and fabrics comprising them
AT80106223T ATE15082T1 (de) 1980-10-13 1980-10-13 Kraeuselfasern aus regenerierter zellulose, verfahren zu deren herstellung und diese fasern enthaltende gewebe.
EP80106223A EP0049710B1 (de) 1980-10-13 1980-10-13 Kräuselfasern aus regenerierter Zellulose, Verfahren zu deren Herstellung und diese Fasern enthaltende Gewebe

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP80106223A EP0049710B1 (de) 1980-10-13 1980-10-13 Kräuselfasern aus regenerierter Zellulose, Verfahren zu deren Herstellung und diese Fasern enthaltende Gewebe

Publications (2)

Publication Number Publication Date
EP0049710A1 true EP0049710A1 (de) 1982-04-21
EP0049710B1 EP0049710B1 (de) 1985-08-21

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EP80106223A Expired EP0049710B1 (de) 1980-10-13 1980-10-13 Kräuselfasern aus regenerierter Zellulose, Verfahren zu deren Herstellung und diese Fasern enthaltende Gewebe

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EP (1) EP0049710B1 (de)
AT (1) ATE15082T1 (de)
DE (1) DE3071017D1 (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014201484A1 (de) 2013-06-17 2014-12-24 Lenzing Ag Hochsaugfähige polysaccharidfaser und ihre verwendung
US10030323B2 (en) 2013-04-05 2018-07-24 Lenzing Aktiengesellschaft Method for the production of polysaccharide fibers with an increased fibrillation tendency
US10196758B2 (en) 2013-06-18 2019-02-05 Lenzing Aktiengesellschaft Polysaccharide fibers and method for producing same
US10221502B2 (en) 2013-04-05 2019-03-05 Lenzing Aktiengesellschaft Polysaccharide fibers and method for the production thereof

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020254931A1 (en) * 2019-06-18 2020-12-24 Grasim Industries Limited Curled shortcut fibres for non-woven fabric and a process for preparation thereof

Citations (5)

* 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
US3720743A (en) * 1970-10-20 1973-03-13 Itt Process for producing high performance crimped rayon staple fiber
AT310923B (de) * 1970-10-22 1973-10-25 Chemiefaser Lenzing Ag Verfahren zur Herstellung von Fasern aus regenerierter Cellulose mit hoher Kräuselung und hoher Dehnung
US4121012A (en) * 1973-07-05 1978-10-17 Avtex Fibers Inc. Crimped, high-strength rayon yarn and method for its preparation
GB2042970A (en) * 1979-02-26 1980-10-01 Avtex Fibers Inc Method of making high wet modulus viscose rayon

Patent Citations (5)

* 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
US3720743A (en) * 1970-10-20 1973-03-13 Itt Process for producing high performance crimped rayon staple fiber
AT310923B (de) * 1970-10-22 1973-10-25 Chemiefaser Lenzing Ag Verfahren zur Herstellung von Fasern aus regenerierter Cellulose mit hoher Kräuselung und hoher Dehnung
US4121012A (en) * 1973-07-05 1978-10-17 Avtex Fibers Inc. Crimped, high-strength rayon yarn and method for its preparation
GB2042970A (en) * 1979-02-26 1980-10-01 Avtex Fibers Inc Method of making high wet modulus viscose rayon

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Chemiefasern/Textilindustrie, Vol. 30, (1980) June, No. 6, Frankfurt am Main, DE M.J. WEICH et al. "Neuentwicklung bei Viskosefasern", pages 492-494. * pages 492,493, under the heading: "Texturierte Viskosefasern" * *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10030323B2 (en) 2013-04-05 2018-07-24 Lenzing Aktiengesellschaft Method for the production of polysaccharide fibers with an increased fibrillation tendency
US10221502B2 (en) 2013-04-05 2019-03-05 Lenzing Aktiengesellschaft Polysaccharide fibers and method for the production thereof
WO2014201484A1 (de) 2013-06-17 2014-12-24 Lenzing Ag Hochsaugfähige polysaccharidfaser und ihre verwendung
US10220111B2 (en) 2013-06-17 2019-03-05 Lenzing Aktiengesellschaft Highly absorbent polysaccharide fiber and use thereof
US10196758B2 (en) 2013-06-18 2019-02-05 Lenzing Aktiengesellschaft Polysaccharide fibers and method for producing same

Also Published As

Publication number Publication date
ATE15082T1 (de) 1985-09-15
EP0049710B1 (de) 1985-08-21
DE3071017D1 (en) 1985-09-26

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