Classifications

• • 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
• • 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
  • D01D5/06—Wet spinning methods
• • 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

Definitions

• the invention relates to a process for the production of cellulose fibers or cellulose filament yarns with improved properties from cellulose by the dry-wet extrusion process with aqueous amine oxides, in particular N-methyl-morpholine-N-oxide, as solvent, in which a) pulp and aqueous amine oxide are added dispersed at elevated temperature in a reactor, with removal of water and shear in 0 a homogeneous solution with a zero shear viscosity in the range of 1000-8000 Pas and a relaxation time in the range of 0.5-80 seconds at 85 ° C, b) the solution at least one Spinning nozzle feeds and deforms, c) the solution jet is transported through a non-precipitating medium with further deformation, and d) the cellulose thread or the yarn filament precipitates in a precipitation bath, separates it from the precipitation bath via a deflecting element and washes in a multi-stage aftertreatment , dries and crosslinked if necessary.
• EP 0 430 926, EP 0 494 852, EP 0 756 025 and WO 94/28 210 describe certain nozzles with different spinning capillary geometry and arrangement.
• WO 96/20 300 deals with the distance between two spinning capillaries and the path between spinning capillary and deflection element in the precipitation bath.
• EP 0 584 318, EP 0 671 492, EP 0 795 052, WO 94/28 218 and WO 96/21 758 describe the different forms of treating the thread family in the gap between the spinneret and the precipitation bath with air having different water contents.
• EP 0 659 219 describes the production of a cellulose fiber with a lower tendency to fibrillation, in that an empirical formula of spinneret hole diameter, spinning mass flow, titer, width of the air gap and moisture content of the blown air should not exceed a value of 10.
• a lower tendency to fibrillation is to be achieved by the fact that the blowing air contains aliphatic alcohols and in EP 0 853 146 by the precipitation taking place in two or more stages.
• the object of the present invention is to create a method with an improved thread-forming process which captures all the relevant variables for thread-forming in a relationship and thus allows a targeted adjustment of fiber / filament properties based on a solution with a defined cellulose concentration, molecular weight and molecular weight distribution.
• the fibers spun according to the invention are intended to allow subsequent crosslinking without significant embrittlement.
• ⁇ D is the expansion viscosity in Pas
• s the expansion speed in s "1 , T 10 the fineness of the material to be spun
• Fiber in dtex v a the withdrawal speed in m / min, p L the density of the solution in g / cm 3 , c Ce ⁇ . the cellulose concentration of the spinning solution in%, D E inlet diameter and D A outlet diameter of the spinning capillary in cm, 1 length of the spinning capillary in cm, a length of the air gap in cm and SV spinning in the air gap, ie the ratio of take-off and spraying speed.
• the expansion viscosity for a spinning solution is determined by the cellulose concentration, the molar mass and molar mass distribution and only changes with the temperature and elongation speed.
• the rate of expansion of the overall process follows
• Concentration also depends on its degree of solvation or state of solution and only after complete solvation, i.e. long release time reaches a minimum final value. Practical spinning solutions are often incompletely solvated for spinning and thus simulate a higher value for the zero shear viscosity or the molar mass. [Cf. Michels Ch. U. Meister F. "Das Textil” 51 (1997) 4 pp. 161-165 and Michels Ch. And Kosan B. "Chemical Fibers Intern.” 50 (2000) 12 pp. 556-561].
• fibers are spun at a stretching speed in the range between 15 and 40 [1 / s] and the fibers are treated in the last stage before drying with a solution which simultaneously contains softening agent, a crosslinking agent and a crosslinking catalyst. After drying and crosslinking, a fiber with a significantly increased wet scrub resistance is obtained with only a slight change in the other fiber parameters.
• filament yarns are spun at a stretching speed in the range 60-100 [l / s], the amine oxide is removed by washing in several stages, dried to a water content> 80% by means of a first heated roller duo and carried by piston diaphragm pumps driven by compressed air motors and spray nozzles onto the thread sheet a defined amount of a mixture of finishing agent and crosslinking agent, dries and crosslinks via a second heated roller duo.
• a filament yarn with significantly increased wet scrub resistance is obtained.
• the method for determining wet scrub resistance has been described in the literature [Mieck KP; Langner H.; Nechwatal A. "Melliand Textile Reports" 74 (1993) p.
• the measure of wet abrasion resistance is the required number of revolutions of a roller of a certain geometry covered with a cellulose fabric, which leads to the breakage of a moistened fiber under defined tension.
• the lyocell fibers have in Depending on their molar mass and orientation, a wet scrub resistance in the range between 10 and 50 scrubbing cycles. From the literature mentioned it also appears that there is sufficient wet scrub resistance if the fiber test results in> 340 scrubbing cycles.
• fibers were produced with the following settings: fiber fineness 1.10 dtex
• the filament sheet was washed, cut into stacks of 50 mm, finished and dried.
• the test revealed the following fiber parameters:
• Cotton-Linters-Zeil-fabric was pretreated enzymatically, pressed to a water content of 50% by mass, dispersed in 2593 g of NMMO with a water content of 25% and with heating, shearing and evaporation of 623 g of water in a homogeneous solution with a zero shear viscosity of 4108 Pas and a relaxation time of 4.9 s transferred at 85 ° C.
• the particle analysis gave a filter value of 90.
• the composition of the solution was 10.6 mass% cellulose, 77.8 mass% NMMO and 11.6 mass% water.
• the cellulose mixture of the solution had a Cuoxam DP of 543 and a non-uniformity of 6.05.
• the application was carried out once by spraying the fiber (B) predried to> 80% water and on the other hand by dipping and pressing using a roller duo (C).
• the fiber test gave the following values:
• 300 g eucalyptus pulp, enzymatically pretreated, pressed to a water content of 45 mass%, are dispersed in 2726 g NMMO with a water content of 30 mass% and with heating, shearing and evaporation of 772 g water in a homogeneous solution (density 1.178 g / cm 3 ) transferred with a zero shear viscosity of 5 081 Pas and a relaxation time of 6.0 s at 85 ° C.
• the particle analysis showed a filter value of 76.
• the composition of the solution was 12.0 mass% cellulose (Cuoxam DP 508, non-uniformity 5.9), 76.3 mass% NMMO and 11.7 mass% water.
• the calculated elongation rate was 21.8 s "1.
• the fiber was washed, finished and dried at 125 ° C. (A).
• A a second series of tests the
• the solution preparation (10.6% cellulose; density 1.16 g / cm 3 at 85 ° C) is carried out analogously to Example 2, the spinning at 84 ° C
• the filaments were wound up as yarn with a fineness of 75 dtex f (58) (A).
• the finish was applied using a precision pump and "fingers".
• the finish contained 10 g / 1 Arkofix (commercial product from 0. AG) and 1 g / 1 magnesium sulfate (B) at the same time.
• the test was carried out using the standard methods as filament yarn ( a, b) as well as after cutting into stacks as fiber A, B.

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• 2000
  • 2000-09-02 DE DE10043297A patent/DE10043297B4/de not_active Expired - Fee Related
• 2001
  • 2001-08-30 CN CNB018147399A patent/CN1211509C/zh not_active Expired - Fee Related
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  • 2001-08-30 AT AT01967050T patent/ATE318947T1/de not_active IP Right Cessation
  • 2001-08-30 WO PCT/DE2001/003334 patent/WO2002018682A1/fr active IP Right Grant
  • 2001-08-30 AU AU2001287542A patent/AU2001287542A1/en not_active Abandoned
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