EP0049710B1 - 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
EP0049710B1
EP0049710B1 EP80106223A EP80106223A EP0049710B1 EP 0049710 B1 EP0049710 B1 EP 0049710B1 EP 80106223 A EP80106223 A EP 80106223A EP 80106223 A EP80106223 A EP 80106223A EP 0049710 B1 EP0049710 B1 EP 0049710B1
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Prior art keywords
viscose
fibers
cellulose
bath
sulfuric acid
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EP80106223A
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English (en)
French (fr)
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EP0049710A1 (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 AT80106223T priority Critical patent/ATE15082T1/de
Priority to DE8080106223T priority patent/DE3071017D1/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.
  • GB-A-2 042 970 there is disclosed a method of making high wet modulus viscose rayon fiber having a multilobular cross section and a characteristic skin-core structure from a modifier-free viscose.
  • An essential difference of the present invention as compared to this publication is the fact that the claimed fiber is a crimped fiber as opposed to the fiber of the GB-patent publication.
  • the spin bath used in the claimed method must contain a larger portion of sodium sulfate than the critical 15% maximum of the spin bath according to the above publication.
  • the zinc sulfate level of the present invention is lower and less broad than the range of 3 to 6% in the British publication.
  • the fibers of the above publication have a structure wherein the core is surrounded by a continuous, uninterrupted skin and a smooth periphery which is in contrast to the structure of the inventive fibers whose skin-core type cross-section can be seen e.g. from Fig. 4.
  • US-A-4. 121 012 discloses a method to prepare a crimped high-strength regenerated cellulose yarn of filaments having a broken skin-core cross-sectional structure.
  • the processing conditions of this process differ appreciable from the process conditions according to the invention, e.g. the ripening values of the viscose and the absence of any modifier added to and incorporated into the viscose according to the present invention.
  • the cross-section of the crimped fiber of the above US - patent is also completely different from the structure of the crimped fiber according to the present invention. The difference can be seen e.g. when looking at Figs. 2 and 3 of the present application.
  • the cross-sections which are shown in Fig. 2 correspond to those of the above US-patent.
  • crimped rayon fibers of the present invention over those in GB-A-2 042 970 is the fact that the inventive fibers are crimped fibers. Yarns prepared from crimped fibers show a definite advantage in cover. Furthermore, the fibers according to the present invention process an evident advantage as compared to fibers of US-A-4. 121 012 since they can be prepared without the use of viscose modifiers (without deteriorating the excellent fiber characteristics). The merits of a modifier-free viscose have been summarized above.
  • 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 denier, as used herein is an average initial wet modulus which is defined as 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 lnstron 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 2.8 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 elininating 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 method of preparation, the spinning bath composition, and the spinning conditions.
  • the viscose contains from 6% to 10% (preferably 7.5 to 9.2%) 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 (preferably 93 to 99% alpha cellulose content) 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 denier per filament (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 a 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.), aftertreated 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 alkali 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 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 in a standardized 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 I 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 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 S0 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 BOD 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)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Claims (19)

1. Ein Verfahren zur Herstellung gekräuselter regenerierter Zellulosefasern mit einem unsymmetrischen, multilobalen Mantel-Kern-Querschnitt, wobei der Kern von einem diskontinuierlich gebrochenen Mantel umhüllt ist, dadurch gekennzeichnet, daß man
a) eine modifiziermittelfreie Viskose bereitet, die etwa 6% bis 10% Zellulose, etwa 4% bis 9% Natronlauge und etwa 28% bis 45% Schwefelkohlenstoff enthält, bezogen auf das Gewicht der Zellulose;
b) die Viskose bis zu einem Natriumchlorid-Salzindex von 5,5 bis 15 and einer Spinnviskosität nach der Kugelfallmethode von 60 bis 110 Sekunden reift;
c) die gereifte Viskose in ein wässriges Spinnbad extrudiert, das etwa 4% bis 8% Schwefelsäure, etwa 0,5% bis 3% Zinksulfat und etwa 16% bis 22% Natriumsulfat enthält und bei einer Temperatur zwischen 40 und 65°C gehalten wird;
d) die Endlosfäden aus dem Spinnbad entfernt, diese durch ein wässriges Verstreckungsbad leitet, das bei einer Temperatur zwischen 85°C und 98°C gehalten wird;
e) die Verweilzeit in dem Spinnbad so einstellt, daß eine Verstreckung der Endlosfäden im Verstreckungsbad von etwa 65% bis 120% erfolgt, wobei die genannten Endlosfäden ein Naßmodul von etwa 5 bis 12 aufweisen;
f) die verstreckten Endlosfäden in Stapelfasern zerschneidet; und
g) die Stapelfasern in Wasser einer Temperatur von 75 bis 100°C ausspült.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die erhaltenen Stapelfasern 15 bis 25 Kräuselungen pro Inch (2,54 cm) aufweisen.
3. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß die Reifung bei Temperaturen zwischen 9°C und 22°C bis zu 30 Stunden erfolgt.
4. Verfahren nach jedem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Viskose etwa 7,5% Zellulose, etwa 7,5% Natronlauge und etwa 31 % Schwefelkohlenstoff enthält, bezogen auf das Gewicht der Zellulose, und daß die Viskose während des Extrudierens einen Salztest zwischen 8,0 und 8,5 liefert.
5. Verfahren nach jedem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß die Viskose etwa 9,2% Zellulose, etwa 6,0% Natronlauge und etwa 30% Schwefelkohlenstoff enthält, bezogen auf das Gewicht der Zellulose, und daß die Viskose während des Extrudierens einen "Natriumchlorid-Salzindex" zwischen 5,7 und 6,3 aufweist.
6. Verfahren nach jedem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß das Spinnbad etwa 6,1 % Schwefelsäure, etwa 2,6% Zinksulfat und etwa 20,9% Natriumsulfat enthält.
7. Verfahren nach jedem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß das spinnbad etwa 5,7% Schwefelsäure, etwa 0,9% Zinksulfat und etwa 20% Natriumsulfat enthält.
8. Verfahren nach jedem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß das Verstreckungsbad 1% bis 4% Schwefelsäure, 0,3% bis 1,2% Zinksulfat und 3% bis 12% Natriumsulfat enthält.
9. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß
a) dis Viskose etwa 7,5% Zellulose, etwa 7,5% Natronlauge und etwa 30% bis 32% Schwefelkohlenstoff enthält und einen Salztest von 6,0 bis 8,5 und eine Kugelfallviskosität von 65 bis 80 Sekunden aufweist;
b) das Spinnbad 5,8% bis 6,5% Schwefelsäure, 2,0% bis 3,0% Zinksulfat und 16% bis 22% Natriumsulfat enthält und bei einer Temperatur von 40 bis 55°C gehalten wird; und
c) das Verstreckungsbad 1,0% bis 4,0% Schwefelsäure, 0,3% bis 1,8% Zinksulfat und 3% bis 12% Natriumsulfat enthält und bei einer Temperatur von 85 bis 95°C gehalten wird, und daß die Endlosfäden in dem Bad etwa 90 bis 120% verstreckt werden.
10. Verfahren nach anspruch 1 und 9, dadurch gekennzeichnet, daß
a) die Viskose etwa 7,5% Zellulose, etwa 7,5% Natronlauge und etwa 31 % Schwefelkohlenstoff enthält und während des Zeitpunkts der Extrudierung einen Salztest von 8,0 bis 8,5 und eine Viskosität nach der Kugelfallmethode von 75 Sekunden aufweist;
b) das Spinnbad etwa 6,1% Schwefelsäure, etwa 2,6% Zinksulfat und etwa 20,9% Natriumsulfat enthält und bei einer Temperatur von etwa 48°C gehalten wird;
c) das Verstreckungsbad etwa 2,5% Schwefelsäure, etwa 1,5% Zinksulfat und etwa 8% Nateriumsulfat enthält und bei etwa 90°C gehalten wird, und daß die Endlosfäden in dem Verstreckungsbad etwa 95 bis 100% verstreckt werden.
11. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß
a) die Viskose etwa 9,2% Zellulose, etwa 6,0% Natronlauge und etwa 29% bis 31% Schwefelkohlenstoff enthält und einen Salzindex von 5,7 bis 6,3 und eine Spinnviskosität nach der Kugelfallmethode von 65 bis 70 Sekunden aufweist;
b) das Spinnbad 5,3% bis 6,0% Schwefelsäure, 0,9% bis 2% Zinksulfat und 17% bis 22% Natriumsulfat enthält und bei einer Temperatur von 50 bis 60°C gehalten wird; und
c) das Verstreckungsbad 1,0% bis 4,0% Schwefelsäure enthält und bei einer Temperatur von 90 bis 95°C gehalten wird, und daß die Endlosfäden in dem Bad etwa 65 bis 85% verstreckt werden.
12. Verfahren nach Anspruch 1 und 11, dadurch gekennzeichnet, daß
a) die Viskose etwa 9,2% Zellulose, etwa 6,0% Natronlauge und etwa 30% Schwefelkohlenstoff enthält und während des Extrudierens einen Salzindex von 5,7 bis 6,3 und eine Kugelfallviskosität von 70 Sekunden aufweist;
b) das Spinnbad etwa 5,7% Schwefelsäure, etwa 0,9% Zinksulfat und etwa 20% Natriumsulfat enthält und bei einer Temperatur von etwa 60°C gehalten wird; und
c) das Verstreckungsbad etwa 2,5% Schwefelsäure, etwa 0,4% Zinksulfat und etwa 8,0% Natriumsulfat enthält und bei einer Temperatur von etwa 93°C gehalten wird, und daß die Endlosfäden in dem Verstreckungsbad etwa 70 bis 75% verstreckt werden.
13. Verfahren nach jedem der Ansprüche 1 bis 12, dadurch gekennzeichnet, daß die modifiziermittelfreie Viskose aus einer sich auflösenden Pulpe mit einem a-Zellulosegehalt von 93 bis 99% hergestellt wird.
14. Gekräuselte, regenerierte Zellulosefaser mit einer Naß-Reißfestigkeit von etwa 1,5 bis 2,7 g pro Denier (17 bis 30,6 N/tex), eine Reißfestigkeit im konditionierten Zustand von etwa 2,8 bis 4,0 g pro Denier (31,7 bis 45,3 N/tex), eine prozentuale Naßausdehnung zwischen etwa 14 und 27%, eine prozentuale Ausdehnung im konditionierten Zustand von 11 bis 22% und einem Naßmodul von 5,0 bis 12,0, weiterhin gekennzeichnet durch einen multilobalen Mantel-Kern-Querschnitt, worin der Kern von einem diskontinuierlich gebrochenen Mantel umhüllt ist, und einem Kräuselungsgrad von 10 bis 30 Kräuselungen vro Inch (25,3 mm), die nach einem Verfahren gemäß jedem der Ansprüche 1 bis 13 hergestellt worden ist.
15. Faser nach Anspruch 14 mit einer Naß-Reißfestigkeit von 2,0 bis 2,3 g pro Denier (22,7 bis 26,4 N/tex), einer Reißfestigkeit im konditionierten Zustand von 3,6 bis 3,8 g pro Denier (40,8 bis 43,1 N/tex), einer prozentualen Naßausdehnung von 25 bis 27%, einer prozentualen Ausdehnung im konditionierten Zustant von 17 bis 20%, einem Naßmodul von 6,0 bis 7,0 und mit 22 bis 25 Kräuselungen pro Inch (25,4 mm), die weiterhin einen durchschnittlichen Polymerisationsgrad von 450 bis 525 aufweist.
16. Faser nach Anspruch 14 mit einer Naß-Reißfestigkeit von 1,7 bis 1,8 g pro Denier (19,3 bis 20,4 N/tex), einer Reißfestigkeit in konditioniertem Zustand von 3,2 bis 3,3 g pro Denier (36,3 bis 37,4 N/tex), einer prozentualen Ausdehnung in nassem Zustand von 15 bis 18%, einer prozentualensAusdehnung in konditioniertem Zustand von 12 bis 14% und einem Naßmodul von 8,0 bis 10,0 mit 10 bis 12 Kräuselungen pro Inch (25,4 mm), die weiterhin einen durchschnittlichen Polymerisationsgrad von 375 bis 400 ausweisen.
17. Textilstoff enthaltend regenerierte Zellulosefasern gemäß jedem der Ansprüche 14 bis 16.
18. Textilstoff aus Baumwolle mit 1 bis 99 Gewichtsprozent (des Textilstoffs) regenerierten Zellulosefasern gemäß jedem der Ansprüche 14 bis 16.
19. Textilstoff aus Polyester mit 1 bis 99 Gewichtsprozent (des Textilstoffs) regenerierten Zellulosefasern gemäß jedem der Ansprüche 14 bis 16.
EP80106223A 1980-10-13 1980-10-13 Kräuselfasern aus regenerierter Zellulose, Verfahren zu deren Herstellung und diese Fasern enthaltende Gewebe Expired EP0049710B1 (de)

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Application Number Priority Date Filing Date Title
AT80106223T ATE15082T1 (de) 1980-10-13 1980-10-13 Kraeuselfasern aus regenerierter zellulose, verfahren zu deren herstellung und diese fasern enthaltende gewebe.
DE8080106223T DE3071017D1 (en) 1980-10-13 1980-10-13 Crimped regenerated cellulose fibers, a method for their preparation and fabrics comprising them
EP80106223A 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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EP80106223A 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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EP0049710B1 true EP0049710B1 (de) 1985-08-21

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WO2020254931A1 (en) * 2019-06-18 2020-12-24 Grasim Industries Limited Curled shortcut fibres for non-woven fabric and a process for preparation thereof

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AT514136A1 (de) 2013-04-05 2014-10-15 Lenzing Akiengesellschaft Polysaccharidfaser mit erhöhtem Fibrillationsvermögen und Verfahren zu ihrer Herstellung
AT514137A1 (de) 2013-04-05 2014-10-15 Lenzing Akiengesellschaft Polysaccharidfaser und Verfahren zu ihrer Herstellung
AT514468A1 (de) 2013-06-17 2015-01-15 Lenzing Akiengesellschaft Hochsaugfähige Polysaccharidfaser und ihre Verwendung
AT514474B1 (de) 2013-06-18 2016-02-15 Chemiefaser Lenzing Ag Polysaccharidfaser und Verfahren zu ihrer Herstellung

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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
GB2042970B (en) * 1979-02-26 1983-01-12 Avtex Fibers Inc Method of making high wet modulus viscose rayon

Cited By (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

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DE3071017D1 (en) 1985-09-26
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