Classifications

• • D—TEXTILES; PAPER
  • D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
  • D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
  • D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
  • D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
• • 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
  • D10B2201/20—Cellulose-derived artificial fibres
  • D10B2201/22—Cellulose-derived artificial fibres made from cellulose solutions
  • D10B2201/24—Viscose
• • 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
  • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
  • Y10T428/00—Stock material or miscellaneous articles
  • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
  • Y10T428/2913—Rod, strand, filament or fiber

Definitions

• Cellulose is the most common and important naturally occurring polymer in the world.
• cellulosic moldings such as paper, blown film, cellophane and sponge cloths
• cellulose fibers are among the important technical products that are used primarily for clothing, as insulating materials and as technical strength carriers.
• Cellulosic fibers, filaments and multifilaments can be obtained in a variety of ways and in various forms, which are also known and familiar to the art.
• the most common methods are the so-called Regenerat method in which cellulose is first reacted and dissolved chemically soluble labile or simply saponifiable derivatives.
• soluble derivatives from which cellulose can be regenerated e.g. Cellulose acetate, cellulose formate or cellulose carbamate known.
• the viscose process the labile derivative is a cellulose xanthate, and the viscose yarns are known as viscose or rayon yarns.
• the solution is pumped through spinnerets, regenerated in a precipitation bath to give viscose filaments, washed and sized (and possibly functionally coated) in one or more post-treatment steps and finally either wound on endless coils or processed into fiber sections.
• the present invention relates to high strength fibers of low total denier viscose multifilament yarn.
• Viscose multifilament yarns for industrial applications often as technical viscose or rayon referred to, are known and are commonly used as a strength carrier for technical products, for example for the reinforcement of elastomeric components and products such as in the form of tire cords, as Schlaucharmtechnik, or as a reinforcing material in belts and conveyor belts.
• High strength, low yarn count multifilament cellulosic yarns are known.
• ultra-high strength low total denier yarns are known from cellulose formate and from a formaldehyde-modified viscose process.
• So in the patent US 6,261,689 Cellulose formate fibers which have been conditioned according to the standard climate defined in EN ISO 20139 (currently DIN EN ISO 139) at a temperature of (20 ⁇ 2) ° C and a relative humidity of (65 ⁇ 2)% and a total titer of 460 dtex and a strength of 76 cN / tex.
• the patent US 3,388,117 describes a formaldehyde-modified viscose process which produces a multifilament viscose yarn consisting of 500 monofilaments and having a total denier of 485 dtex. After conditioning in a climate of 20 ° C and 65% relative humidity, a strength of 78 cN / tex is measured, said strength was determined not on the multifilament yarn but on an undisclosed number of individual filaments, which were removed from the multifilament.
• Patent GB 685,631 describes rayon yarns, ie 100 multifilament yarns of 100 individual filaments with a low total denier of 100 den (110 dtex) but with a conditioned tenacity of only 2.3 g / den (20.4 cN / tex). and with an oven-dry strength of 2.9 g / den (25.6 cN / tex).
• GB 685,631 discloses yarns having a yarn count of 400 denier (440 dtex) with 260 filaments and moderate strengths of 4.1 g / den (36.2 cN / tex) in the conditioned and 5.3 g / den (respectively). 46.8 cN / tex) in the oven-dried viscose multifilament yarn.
• the object of the present invention is to provide a viscose multifilament yarn which is produced without formaldehyde yet has high strength measured on the conditioned multifilament yarn.
• a viscose multifilament yarn produced without the use of formaldehyde wherein the viscose multifilament yarn a degree of crystallinity in the range of 15% to 40% and after conditioning in standard atmosphere according to DIN EN ISO 139-1: 2005 at a temperature of 20 ⁇ 2 ° C and a relative humidity of 65 ⁇ 2% in a conditioning time of ⁇ 16 h to an equilibrium moisture content of 13 ⁇ 1% a yarn titer in the range of ⁇ 150 dtex to ⁇ 1100 dtex and a tensile strength in the range of ⁇ 45 cN / tex to ⁇ 55 cN / tex.
• the viscose multifilament yarn according to the invention is produced without the use of formaldehyde and nevertheless shows a tensile strength measured on the viscose multifilament yarn in the range from ⁇ 45 cN / tex to ⁇ 55 cN / tex.
• the viscose multifilament yarn according to the invention is for a person skilled in the art is shown by the fact that even the inventors can not explain why the viscose multifilament yarn according to the invention with its property combination consists of a yarn denier in the range of ⁇ 150 dtex to ⁇ 1100 dtex and Degree of crystallinity in the range of 15% to 40% has a measured on the viscose multifilament yarn tensile strength in the range of ⁇ 45 cN / tex to ⁇ 55 cN / tex.
• the degree of crystallinity of the formaldehyde-made viscose multifilament yarn is US 3,388,117 at 45% and thus considerably higher.
• the term "conditioned" means that the viscose multifilament yarn according to the invention is stored in the abovementioned standard climate until the yarn has reached its equilibrium moisture content corresponding to the standard climate, which is 13 ⁇ 1% by weight, and therefore its weight not changed anymore. For this purpose, a conditioning time in the above-mentioned standard climate of ⁇ 16 h is required.
• the degree of crystallinity of the viscose multifilament yarn of the present invention is determined by wide angle X-ray diffraction (WAXS), as in Hermans, PH, Weidinger, A., Textile Research Journal 31 (1961) 558-571 described, wherein the determined values have an estimated maximum error of ⁇ 1.5% points.
• WAXS wide angle X-ray diffraction
• the viscose multifilament yarn according to the invention has a degree of crystallinity in the range from 20% to 35%, a yarn denier in the range from ⁇ 170 dtex to ⁇ 900 dtex and a tensile strength in the range from ⁇ 45 cN / tex to ⁇ 55 cN / tex on.
• the viscose multifilament yarn according to the invention has a degree of crystallinity in the range of 24% to 30%, a yarn titer in the range of ⁇ 200 dtex to ⁇ 840 dtex and a tensile strength in the range of ⁇ 48 cN / tex to ⁇ 53 cN / tex on.
• the viscose multifilament yarn according to the invention has a crystallite width in the range of 2.5 nm to 5.0 nm, more preferably in the range of 3.0 nm to 4.5 nm, and a crystal height in the range of 9.0 nm to 13.0 nm, more preferably in the range of 10 nm to 12 nm on.
• the crystallite width is determined from the reflex of the L (1-10) crystal plane and the crystal height from the reflex of the L (004) crystal plane.
• High-strength cellulosic fibers which can be spun from formaldehyde-modified viscoses / precipitation baths and correspondingly more highly drawn, show significantly larger L (004) reflections.
• the discontinued product Cordenka EHM ® showed a crystallite height of 15.0 nm.
• the viscose multifilament yarn according to the invention has a birefringence ⁇ n ⁇ 10 4 in the range from 300 to 450, particularly preferably in the range from 330 to 420.
• the birefringence ⁇ n is measured with the aid of an interference microscope [ J. Lenz, J. Schurz, D. Eichinger, Lenzinger Reports 1994, 9, p.
• the viscose multifilament yarn according to the invention has a filament titer in the range of 1.2 and 4.0 dtex.
• the viscose multifilament yarn according to the invention has a filament titer in the range of 2.4 and 3.0 dtex.
• the viscose multifilament yarn according to the invention has an elongation at break in the range of ⁇ 5% and ⁇ 20%.
• the viscose multifilament yarn according to the invention has an elongation at break in the range of ⁇ 6% and ⁇ 15%.
• the following table gives an exemplary overview of inventive viscose multifilament yarns with a conditioned yarn denier of 204 dtex to 1013 dtex.
• the viscose multifilament yarns according to the invention were obtained by the abovementioned modifications of the preparation process described in Example 2 of GB 685,631 and in the normal climate according to DIN EN ISO 139-1: 2005, ie at a temperature of 20.0 ° C. and at a relative atmospheric humidity of 65%, conditioned and the textile data yarn count, maximum tensile strength, tensile strength and elongation at break in the conditioned state according to DIN EN ISO 2062: 2009 measured under the conditions already described.
• the tensile strength is called denomination-related maximum tensile strength and elongation at break are referred to as maximum tensile elongation at break.
• the table contains values for the degree of crystallinity determined by wide angle X-ray diffraction (WAXS), values for the crystallite width determined from the L (1-10) crystal plane reflex and values for the crystal height from the reflex of the L (004) crystal plane and a value for the birefringence ⁇ n ⁇ 10 4 measured by interference microscopy.
• WAXS wide angle X-ray diffraction
• the tensile strength of a selected number of individual filaments taken from a multifilament yarn is greater than the tensile strength measured on the multifilament yarn.
• a tensile strength of 60.4 cN / tex and an elongation at break are obtained of 11.8%.
• the tensile strength measured on the conditioned monofilaments is 20% higher and the elongation at break 28% higher than the corresponding values measured on the viscose multifilament yarn of Example 3.
• the following table shows the difference between textile data of the same yarn example, which are obtained in conditioned (DIN EN ISO 139-1: 2005) or in oven-dry measurements: Measuring conditions / tested parameters Conditioning> 16 h at 20 ° C and 65% relative humidity Oven-dry (2 h at 105 ° C) Garntiter [dtex] 646 560 filament 240 240 Maximum tensile strength [N] 32.2 36.0 Tensile strength [cN / tex] 49.8 63.0 Elongation at break [%] 8.62 8.16
• the viscose multifilament yarn according to the invention has a yarn count in the range of ⁇ 150 dtex to ⁇ 1100 dtex, preferably from ⁇ 170 dtex to ⁇ 900 dtex, and more preferably in front ⁇ 200 dtex to ⁇ 840 dtex.
• the viscose multifilament yarns according to the invention have a yarn count in the range of ⁇ 150 dtex to ⁇ 1100 dtex or a yarn count in the range of ⁇ 170 dtex to ⁇ 900 dtex or a yarn count in the range of ⁇ 200 dtex to ⁇ 840 dtex and contain filaments having a filament denier between 1.2 and 4.0 dtex, more preferably between 2.4 and 3.0 dtex.
• such viscose multifilament yarns according to the invention are not only suitable for the production of thin cords, but also give cords of very high fatigue resistance.
• An example of this is high-tenacity viscose multifilament yarn of the invention having a conditioned dtex of 800 dtex with 300 filaments (800 dtex f300 rayon).
• the nature or presentation of the cellulosic fibers is not limited.
• the viscose multifilament yarn of the present invention be processed as such or as a fiber short to a cord, to a woven or knitted fabric, wherein the cord or the fabric can be used to reinforce eg tires.
• the viscose multifilament yarn of the present invention can be used to make a cord.
• the cord containing the viscose multifilament yarn of the present invention can be made into a fabric.
• the fabric may be impregnated and the impregnated fabric used to make a tire. It is also possible to use the cord containing the viscose multifilament yarn according to the invention directly for the production of a tire.
• the viscose multifilament yarn of the present invention may serve as a reinforcing material for synthetic and natural elastomers or for other synthetic or renewable raw materials based materials, for example, thermoplastic and thermosetting plastics.
• materials which may be elastomeric, thermoplastic or duromeric materials include, for example, natural rubber, other poly (isoprene) s, poly (butadiene) s, polyisobutylenes, butyl rubber, poly (butadiene-co-styrene) s, poly (butadiene -coacrylonitrile) s, poly (ethylene-co-propylene) s, poly (isobutylene-co-isoprene) s, poly (chloroprene) s, polyacrylates, polyamide, polyesters, polylactic acid, polycarbonates, polyglucans, polyurethanes, polysulfides, silicones, polyvinyl chloride , Poly (ether-ester

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• 2014
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