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
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
  • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
  • D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
  • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
  • D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
  • D06M13/272—Unsaturated compounds containing sulfur atoms
  • D06M13/278—Vinylsulfonium compounds; Vinylsulfone or vinylsulfoxide compounds

Definitions

• the present invention relates to a new cellulose fiber and a method for producing this cellulose fiber.
• a tertiary amine oxide in particular N-methylmorpholine-N-oxide (NMMO)
• NMMO N-methylmorpholine-N-oxide
• a characteristic property of Lyocell fibers is their pronounced tendency to fibrillate when wet. Fibrillation is understood to mean breaking open the wet fiber in the longitudinal direction under mechanical stress in the wet state, as a result of which the fiber is given a hairy, furry appearance. The reason for the fibrillation is believed to be the fiber consists of fibrils arranged in the direction of the fibers, between which there is only a small amount of crosslinking.
• WO 92/14871 describes a method for producing a fiber with a reduced tendency to fibrillation. This is achieved in that all baths with which the freshly spun fiber comes into contact before the first drying have a pH of a maximum of 8.5.
• WO 92/07124 also describes a method for producing a fiber with a reduced tendency to fibrillation, according to which the freshly spun, that is to say not yet dried, fiber is treated with a cationizable polymer.
• a polymer with imidazole and azetidine groups is mentioned as such a polymer.
• treatment with an emulsifiable polymer e.g. Polyethylene or polyvinyl acetate, or crosslinking with glyoxal.
• Lyocell fibers can be improved by chemical crosslinking.
• EP-A-0 538 977 describes the crosslinking of lyocell fibers with chemical reagents which can react with cellulose, both in the never-dried state, that is to say during fiber production, and also in the dried state, that is to say essentially during the textile finishing of the textile fabrics.
• crosslinking reagents cited as examples in the above-mentioned patent application EP-A - 0 538 977 have, as crosslinkable groups, halogen-substituted, nitrogen-containing ring structures which are capable of reacting with the hydroxyl groups of cellulose under alkaline conditions. Compounds with vinyl sulfone groups or their precursors are also described. These compounds also react essentially only when alkali is added or require alkali as neutralizing reagent for split off acids.
• a disadvantage is that in the reaction of the halogenated, nitrogen-containing rings or the vinyl sulfones or their precursors, salts are formed which then have to be washed out of the fiber, and excess chemicals which have not reacted with the cellulose fiber must also be washed out. This means that a further post-treatment step is necessary in a continuous fiber production process, which causes further investment costs and operating costs and additionally brings with it problems with contaminated wastewater.
• WO 94/24343 by the applicant proposes similar procedures for crosslinking the Ly ⁇ cell fiber against fibrillation, where the use of alkaline buffers and radiation with electromagnetic waves are described as being particularly advantageous.
• WO 94/20656 describes that the fibrillation of Lyocell fibers by crosslinking with conventional crosslinking chemicals, which is usually used to improve the Crease angle of cellulose textiles are used without reducing the dyeability of the fibers if the crosslinking is carried out in the presence of flexible, linear polymers.
• conventional crosslinking chemicals which is usually used to improve the Crease angle of cellulose textiles are used without reducing the dyeability of the fibers if the crosslinking is carried out in the presence of flexible, linear polymers.
• conventional N-methylol resins low in formaldehyde
• the usual acidic catalysts are used. The method is described as leading to success for both the dried and the never dried fiber.
• dried substrates such as fibers, fabrics, films and paper
• aqueous, 5-25% strength solutions of the crosslinking agent and 4-35% strength aqueous solutions of alkali either first with crosslinking agent and then with alkali , or vice versa, first with alkali and then with crosslinker.
• the crosslinker with the alkali can be applied from a bath and a treatment at high temperature can then be carried out for the crosslinking.
• intermediate drying can be carried out between the treatment with crosslinking agent and the treatment with alkali.
• Alkaline metal hydroxides, alkali metal carbonates and bicarbonates, and quaternary ammonium bases such as trimethylammonium hydroxide are used as alkaline compounds.
• the reaction times given are 10 minutes at room temperature or shorter residence times at a higher temperature, for example 3 minutes at 150 ° C. After the reaction, the substrate must be washed free of alkali.
• the present invention thus aims to provide a process for the production of Lyocell fibers with which fibers can be produced which have a predetermined tendency to fibrillate.
• the process according to the invention for the production of cellulose fibers by the amine oxide process in which process a solution of cellulose in an aqueous tertiary amine oxide is spun into fibers and the fibers are brought into contact with a crosslinking agent, is characterized in that a sulfonium compound of the formula (I ) CH-CH-.Z, y 2 2
• OW is the residue of a polybasic acid in salt or acid form
• R CH-CH-OW, alkyl, in particular C 1 -C.alkyl, aryl, substituted alkyl or a heterocycle, is used.
• An internal salt of dialkali-tris ( ⁇ -sulfatoethyl) sulfonium, in particular the inner salt of disodium tris ( ⁇ -sulfatoethyl) sulfonium, is preferably used as the sulfonium compound of the formula (II) in the process according to the invention.
• the fibers can be brought into contact with the crosslinking agent both in the never-dried state and in the dried state, although it is preferred to use the fibers in the never-dried state, for example freshly spun, to be brought into contact with the crosslinking agent.
• the fibers are preferably treated with a base after they have been brought into contact with the crosslinking agent, and the fibers can be dried before treatment with the base.
• a particularly advantageous embodiment of the process according to the invention consists in treating the fibers with a base and simultaneously bringing them into contact with the crosslinking agent, the base and crosslinking agent being in a molar ratio of essentially 3: 1 (base: crosslinking agent).
• the fibers are then dried. It has been found that no washing of the fibers is required in this embodiment of the method according to the invention. This is advantageous in that one step in the manufacturing process can be saved.
• the fibers are best brought into contact with an aqueous solution which contains trisSS in a concentration of 0.3 to 25% by mass, preferably 0.5 to 5% by mass.
• the base is contained in the aqueous solution in 0.8 to 100 molar, preferably in 2.5 to 3.5 molar amount, based on trisSS.
• alkali metal hydroxides, alkali metal carbonates and bicarbonates, quaternary ammonium bases and polymeric amines are used as the base. It has also been found that buffer solutions with a pH in the range from 5 to 12, preferably from 7 to 9, can also be used according to the invention.
• the invention also relates to cellulose fibers with a predetermined tendency to fibrillation, which are obtainable by the process according to the invention.
• the invention further relates to the use of a sulfonium compound of the formula (I)
• R_, Z and Y ⁇ have the meaning given above, and / or a sulfonium compound of the formula (II)
• OW and R_ have the meaning given in claim 1, for the treatment of fibers which have been produced by the amine oxide process and of yarns and fabrics made of fibers which have been produced by the amine oxide process.
• the invention also relates to the use of an inner salt of dialkali tris ( ⁇ -sulfatoethyl) sulfonium for the treatment of fibers which have been produced by the amine oxide process and of yarns and woven fabrics made of fibers which have been produced by the amine oxide process.
• Dialkali-Tris (ß-sulfatoethyl) sulfoniums, wherein base and crosslinking agent are in a molar ratio of essentially 3: 1 (base: crosslinking agent), for the treatment of fibers by the amine oxide process and yarns and fabrics made from fibers made by the amine oxide process.
• the freshly spun, never-dried fiber strand or the never-dried fiber flake can first be impregnated with the solution of trisSS and, after being squeezed to a moisture content of 100 to 150%, impregnated with the base solution, whereby the order of treatment can also be reversed. After a residence time of about 10 minutes at room temperature, washing and drying can be carried out.
• the process according to the invention can be carried out in one step, the fiber being treated simultaneously with the solution of trisSS and small amounts of base in a one-step process.
• alkaline compounds such as alkali metal bicarbonates
• heat treatment of the impregnated fiber is then required.
• the temperature treatment can be achieved by drying at temperatures of at least 60 ° C. If the molar ratio of base to triSS is not greater than 3: 1, subsequent washing is not necessary.
• the treatment according to the invention with the crosslinking agent can be carried out before, simultaneously with or after a dyeing process.
• the sulfonium compounds mentioned can, for example, be added to the alkaline dyebath.
• a conventional cellulose fiber of the Lyocell genus has about 50 fibrils per 0.276 mm fiber length.
• a conventional cellulose fiber of the genus Modal which is known to have no tendency to fibrillate and was used as a comparison, shows 1 to 2 fibrils.
• Table 1 shows the concentrations of trisSS in g / 1.
• concentration of the sodium hydroxide solution is given in g NaOH / 1.
• Examples 5 to 8 show that the fibril count decreases with increasing concentration of sodium hydroxide solution, so that the fiber produced fibrillates less.
• trisSS according to the invention it is thus possible to control the tendency of the lyocell fiber to fibrillate via the concentration of alkali.
• Table 2 shows the trisSS concentrations in g / 1.
• concentration of the base is given in g / 1.
• Examples 9 to 24 show the influence of the base concentration on the reduction in fibrillation. Even with a molar ratio of base to crosslinking agent of 3: 1, fibrillation is eliminated when NaOH is used as the alkali component (see Examples 23, 24), and it is not necessary to use higher amounts of NaOH (see Examples 15-18).

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• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
• Materials For Medical Uses (AREA)
• Artificial Filaments (AREA)
• Polysaccharides And Polysaccharide Derivatives (AREA)

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Publications (1)

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Citations (3)

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• 1995
  • 1995-08-18 AT AT0140295A patent/AT402642B/de not_active IP Right Cessation
• 1996
  • 1996-08-16 AU AU66955/96A patent/AU712681B2/en not_active Ceased
  • 1996-08-16 CA CA002202141A patent/CA2202141A1/en not_active Abandoned
  • 1996-08-16 CN CN96191144.1A patent/CN1165544A/zh active Pending
  • 1996-08-16 EP EP96926961A patent/EP0783602B1/de not_active Expired - Lifetime
  • 1996-08-16 DE DE59600086T patent/DE59600086D1/de not_active Expired - Fee Related
  • 1996-08-16 JP JP9508734A patent/JPH10507497A/ja active Pending
  • 1996-08-16 WO PCT/AT1996/000147 patent/WO1997007267A1/de active Application Filing
  • 1996-08-16 AT AT96926961T patent/ATE162858T1/de not_active IP Right Cessation
  • 1996-08-16 BR BR9606586A patent/BR9606586A/pt not_active Application Discontinuation
• 1997
  • 1997-04-17 NO NO971754A patent/NO971754D0/no unknown

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