EP0888467B1 - Verfahren zur herstellung von cellulosischen fasern mit verringerter fibrillierungsneigung - Google Patents

Verfahren zur herstellung von cellulosischen fasern mit verringerter fibrillierungsneigung Download PDF

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Publication number
EP0888467B1
EP0888467B1 EP97915374A EP97915374A EP0888467B1 EP 0888467 B1 EP0888467 B1 EP 0888467B1 EP 97915374 A EP97915374 A EP 97915374A EP 97915374 A EP97915374 A EP 97915374A EP 0888467 B1 EP0888467 B1 EP 0888467B1
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EP
European Patent Office
Prior art keywords
range
tertiary amine
amine oxide
additive
process according
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Expired - Lifetime
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EP97915374A
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German (de)
English (en)
French (fr)
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EP0888467A1 (de
Inventor
Abdulmajid Hashemzadeh
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Akzo Nobel NV
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Akzo Nobel NV
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    • 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
    • D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/08—Organic compounds
    • 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
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
    • 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
    • D06M13/322—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 nitrogen
    • D06M13/388—Amine oxides

Definitions

  • the invention relates to a method for reducing the tendency to fibrillation of cellulosic fibers by spinning a solution of cellulose in a tertiary amine oxide, in particular in N-methylmorpholine-N-oxide (NMMO).
  • NMMO N-methylmorpholine-N-oxide
  • WO-A1-95 / 16063 describes a method in which in the precipitation bath and / or in the wash baths a surfactant is added.
  • the object of the invention is therefore to provide a method to put that without changes to the known, with high Optimized spinning, stretching and precipitation bath technology gets along and if possible only such chemicals needed as used in the above mentioned process become.
  • a manufacturing method of cellulosic fibers by spinning a possibly still water and optionally a stabilizer-containing solution of cellulose in a tertiary amine oxide in a coagulation bath, washing, and Drying the fibers, which is characterized in that one the fibers after leaving the precipitation bath and before washing with a solution containing a tertiary amine oxide and with heat treated, the solution containing the tertiary amine oxide a concentration of the tertiary amine oxide in the range of about Has 40 to 80 wt.% And possibly an additive in a concentration range contains from about 0.5 to 10% by weight, and wherein heat treatment in a temperature range from about 60 to 250 ° C takes place, either simultaneously with or afterwards to treatment with the one containing the tertiary amine oxide Solution, or that one still containing tertiary amine oxide Fibers after leaving the coagulation bath only the heat treatment submits.
  • the solution containing the tertiary amine oxide and / or an additive can organic cosolvents such as Dimethylformamide or contain dimethyl sulfoxide, but is preferably aqueous.
  • organic cosolvents such as Dimethylformamide or contain dimethyl sulfoxide, but is preferably aqueous.
  • N-methylmorpholine-N-oxide is preferred as the tertiary amine oxide (NMMO) used.
  • An embodiment of the invention consists in the simultaneous Treatment of the fibers coming from the precipitation bath with the tertiary amine oxide, preferably NMMO-containing solution and heat.
  • the tertiary amine oxide preferably NMMO-containing solution and heat.
  • heat and mass transfer processes can in effect the solution turbulence or pressure waves e.g. by ultrasound be generated.
  • the treatment temperature is preferably in the range of about 70 to 120 ° C, particularly preferably in the range of about 80 to 90 ° C.
  • Another embodiment of the invention is treatment of the fibers coming from the precipitation bath with the one tertiary Amine oxide, preferably NMMO-containing solution in one Temperature range from about 20 to 25 ° C and subsequent heat treatment. All substances are suitable as heat transfer media, who alone or in a mixture are capable of the occurrence of the reduced tendency to fibrillation is necessary Heat and mass transfer processes are sufficiently quick to accomplish and towards cellulose and the tertiary Amine oxide are chemically inert. Hot gases have this suitability such as. Nitrogen, water vapor or air. Is preferred hot air in a temperature range of about 120 to 250 ° C, especially in a temperature range of about 130 to 180 ° C used. After the heat treatment, the fibers become known Way washed and dried.
  • the one tertiary Amine oxide preferably NMMO-containing solution in one Temperature range from about 20 to 25 ° C and subsequent heat treatment. All substances are suitable as heat transfer media, who alone or in a mixture are capable of the occurrence of the reduced tendency to fibr
  • a particularly preferred embodiment of the invention exists in blowing the fibers coming out of the precipitation bath with a hot gas such as Air or nitrogen, the gas preferably a temperature in the range of about 120 to 250 ° C, particularly preferably in the range of about 150 to 180 ° C. has a tertiary amine oxide without prior treatment containing solution. Then the fibers are known Way washed and dried.
  • a hot gas such as Air or nitrogen
  • the gas preferably a temperature in the range of about 120 to 250 ° C, particularly preferably in the range of about 150 to 180 ° C. has a tertiary amine oxide without prior treatment containing solution.
  • the precipitation bath usually with an NMMO content in the range of about 30 to 65% by weight.
  • the different values come e.g. through different spinning speeds and precipitation bath compositions.
  • the invention is The method can be adapted in that a more intensive or a less intensive treatment with heat and possibly with the solution containing the tertiary amine oxide and optionally an additive takes place, the smaller or the larger the NMMO content of fiber coming from the precipitation bath.
  • the fiber becomes longer after the precipitation bath and / or heat treat hotter and even more tertiary Use solution containing amine oxide with less NMMO Fiber has left the precipitation bath, whereas the shorter and / or the less hot heat treated and one less uses solution containing tertiary amine oxide, the more NMMO contains the fiber after leaving the coagulation bath.
  • the Treated fibers After leaving the precipitation bath and before washing, the Treated fibers with a solution containing a tertiary amine oxide.
  • concentration of those containing the tertiary amine oxide Solution of tertiary amine oxide is preferably in the range from about 60 to 80% by weight if no additive is used.
  • the concentration of the solution containing the tertiary amine oxide tertiary amine oxide is preferably in the range of about 40 up to 80% by weight if the solution additionally contains an additive.
  • an additive in the tertiary amine oxide containing solution is advantageous if there is a risk that the cellulosic filaments during the heat treatment glue together.
  • the additive then acts to glue individual Filaments and increases the wettability of the fibers.
  • P polyvinyl pyrrolidone
  • One embodiment of the invention with an additive consists in that the fibers with an aqueous, the tertiary amine oxide and the solution containing additive are treated.
  • the temperature this solution is preferably in the range of about 20 to 25 ° C.
  • the fibers are joined with another one treated solution containing tertiary amine oxide, the Solution preferably a temperature in the range of about 70 to 120 ° C, particularly preferably in the range of about 80 to 90 ° C. and finally washed and dried in a known manner.
  • the fibers first contain one containing the additive Solution and then with the containing the tertiary amine oxide Solution are treated, the concentration of the tertiary Amine oxide in the solution preferably in the range of about 47 to 80% by weight.
  • Both solutions are preferably aqueous, can but contain the mentioned cosolvents.
  • the temperature of both Solutions are in the range of about 20 to 25 ° C.
  • the fibers are washed with a hot gas such as Air or Treated nitrogen, the gas preferably a temperature in the range of about 120 to 250 ° C, particularly preferably in Has a range of about 130 to 150 ° C and finally in the known Way washed and dried.
  • a third embodiment of the invention with additive exists in that the fibers with a preferably aqueous, the tertiary Amine oxide and the additive-containing solution treated which have a temperature in the range of about 70 to 120 ° C, preferably in the range of about 80 to 90 ° C. Subsequently the fibers are washed in a known manner and dried.
  • the solution containing the additive can in principle be used with any Device can be carried out that is capable of Sufficiently provide fibers with the solution mentioned.
  • the solution should cover the fiber surface as completely as possible.
  • sprinklers or spray devices for Get involved are examples that are not exhaustive.
  • the treatment times of the fibers in the tertiary amine oxide and optionally the solution containing the additive is in the range of about 0.1 to 10 seconds, preferably in the range of about 1 to 5 Seconds.
  • the treatment times of the fibers in the heat treatment zone are preferably in the range of about 0.2 to 10 seconds, particularly preferably in the range of about 2 to 6 seconds.
  • Fibers can not only be integrated as already described in the spinning process after the precipitation bath and before washing take place, but also on washed and possibly dried fibers or on washed and, if necessary, dried from them or on unwashed textile fabrics such as Fabrics, knitwear, nonwovens or thread-laid fabrics, furthermore on yarns, fiber sheets and fiber tapes. Staple fibers, Short cut fibers or flakes and blended yarns Cellulose and synthetic fibers are treated. To this Purpose are the fibers or fiber products mentioned with a a solution containing tertiary amine oxide and with heat treated, the temperature of the heat treatment in the range from about 60 to 250 ° C.
  • the concentration of the tertiary Amine oxides are preferably in the range from about 40 to 80% by weight in the range of about 45 to 75% by weight.
  • which is the tertiary amine oxide containing solution can be in a concentration range of about 0.5 to 10 wt.% Contain an additive.
  • the heat treatment can either be with or after treatment in which contains the tertiary amine oxide and optionally the additive Solution. Then the fibers or the products made from it and already described in washed and dried in a known manner.
  • the additive fulfills the task already described and will selected from the group of additives already described.
  • Polyvinylpyrrolidone is preferably used.
  • the solution containing the tertiary amine oxide and / or an additive can an organic cosolvent such as Dimethylformamide or contain dimethyl sulfoxide, but is preferably aqueous.
  • N-methylmorpholine-N-oxide is preferred as the tertiary amine oxide used.
  • Products with the additive can also be used before treatment with the solution containing the tertiary amine oxide occur.
  • concentration ranges for those containing the additive and for those containing the tertiary amine oxide Solution used as already for the treatment of Fibers after felling and before washing were described.
  • the treatment times of the washed and possibly dried fibers and washed and, if necessary, dried or unwashed products lie with a range of about 0.2 to 60 seconds higher overall than in the treatment of Fibers immediately after the precipitation bath.
  • High titers and fiber products with a dense arrangement of the fibers require longer Treatment times as low titers and products with one loose fiber structure. Under otherwise identical conditions the longer treatment times are necessary, the larger the Degree of polymerization of the cellulose used.
  • the wet scrub test is used to measure the tendency of individual threads to fibrillate Wet scrub test apparatus shown schematically in FIG. Around the tendency to fibrillation of the fiber products already described To judge, the wet scrub test with threads carried out, which were removed from the named products.
  • the wet scrub test consists essentially of the Elements (1) to (6), which are explained below:
  • the Thread (2) is fixed in a PVC block (1).
  • the abrasion is produced in that the thread (2) with a 25th Revolutions per minute rotating assembly is guided, the from a attached to a glass rod (5) with 6mm diameter Ceramic rod (4) with a diameter of 2.5 mm.
  • By dripping with water (3) is tightened by a weight (6) of 3 g Thread kept wet.
  • the wet scrub test was for 1 minute carried out.
  • the one defined with the apparatus described and reproducible fibrillation was performed on a Scale with the marks 1 to 6 by microscopic evaluation of the scrubbed, about 3 mm long fiber area assessed.
  • Primary fibrillation means that only on the fiber surface Fibrils are observed.
  • Secondary fibrillation means that the fibrils are also in deeper layers of the filaments can be observed. The stronger the secondary fibrillation progresses, the longer and the fibrils become thicker.
  • the fibers treated according to the invention surprisingly showed a significantly reduced tendency to fibrillation.
  • the fibrillation of fibers after felling and before washing treated were given a grade of 2-3. dried fibers or washed and possibly made from them dried or unwashed fiber products received afterwards of treatment 3 - 4.
  • the invention is not based on the use of any particular one Degree of polymerization DP of the cellulose raw material limited. Rather you can use pulp or cotton linters with a DP in the range of about 400 to 7000 individually or as Mixture of celluloses with high and low degrees of polymerization use.
  • the invention is not based on the use of a certain stabilizer in the spinning solution.
  • a certain stabilizer in the spinning solution.
  • Much more All fabrics can be used that act as stabilizers suitable, e.g. Pyrogallol, gallic acid or propyl gallate.
  • the invention is not limited to any particular cellulosic Fiber type limited, but includes all cellulosic Fiber types such as Continuous filaments or fibers, staple or Short cut fibers and blended yarns made from cellulosic and synthetic Fibers. Flake can also be treated.
  • the invention is not limited to the fact that the fibers or a fabric made from it under one certain mechanical stress must be. Rather you can the fibers or the textile fabrics made from them without mechanical tension or in a mechanical state Voltage can be used.
  • the invention is not limited to the use of any one tertiary amine oxide limited, but preferred N-methylmorpholine-N-oxide (NMMO).
  • NMMO N-methylmorpholine-N-oxide
  • a fiber containing 55% by weight of N-methylmorpholine-N-oxide (NMMO) has left the precipitation bath, is pulled through a treatment bath, in which there is a solution of 78% by weight NMMO in water, which is kept at 80 ° C.
  • the fiber speeds and the dimensions of the treatment bath are adjusted so that a fiber residence time of 3 ⁇ 1 seconds results.
  • the fiber in a known manner to a residual content washed and dried by ⁇ 1% by weight NMMO.
  • the tendency to fibrillation of the fiber treated in this way received the Grade 2.
  • the tensile strength of the fiber treated according to this example is 38 cN / tex (untreated: 40 cN / tex), the module at 5% Elongation 23 cN / tex (untreated: 24 cN / tex) and the elongation at break 11% (untreated 11%). Since the measurement error range of the just mentioned Fiber data is ⁇ 10%, the results show that the treatment according to the invention is capable of fibrillation reduce while maintaining the mechanical fiber properties.
  • a fiber that has left the precipitation bath with 55% by weight NMMO is drawn through a treatment bath in which there is a solution of 65 wt.% NMMO is in water, which is kept at 90 ° C. becomes.
  • the fiber speed and the dimensions of the treatment bath are set so that a fiber residence time of about 4 seconds results.
  • the fiber in known Washed to a residual content of ⁇ 1 wt% NMMO and dried. The tendency to fibrillation of those treated in this way Fiber received a grade of 2-3.
  • a fiber that has left the precipitation bath with 55% by weight NMMO is drawn through a treatment bath in which there is an aqueous Solution of 48 wt.% NMMO and 2 wt.% Polyvinyl pyrrolidone (PVP), which has a temperature of 22 ⁇ 3 ° C.
  • PVP Polyvinyl pyrrolidone
  • the fiber drawn through a second bath containing a solution of 65% by weight Contains NMMO in water, which is kept at 90 ° C.
  • the fiber speed and the dimensions of the second treatment bath are set so that a fiber dwell time of about 4 Seconds results.
  • the fiber in known Washed and dried to a residual content of ⁇ 1 wt.% NMMO.
  • the tendency to fibrillation of those treated in this way Fiber received a grade of 2-3.
  • a fiber that has left the precipitation bath with 55% by weight NMMO is drawn through a treatment bath that has a temperature of 20 ⁇ 3 ° C.
  • the fiber speed and the dimensions of the treatment bath are set so that a fiber dwell time of about 1.5 ⁇ 0.5 seconds results.
  • the length of the Hot air path is set so that a fiber dwell time results in the hot air zone of 3.5 ⁇ 0.5 seconds.
  • the fiber is known to a residual content washed and dried by ⁇ 1% by weight NMMO.
  • the tendency to fibrillation of the fiber treated in this way received the Grade 2 - 3.
  • a fiber that has left the precipitation bath with 55% by weight NMMO is with an aqueous solution of 78 wt.% NMMO with a Drip device sprinkled.
  • the NMMO solution has a temperature of 85 ⁇ 5 ° C.
  • the thread speed and the length the sprinkler section are set so that a dwell time results in a sprinkling distance of 3 ⁇ 1 seconds.
  • the fiber is kneaded in a known manner Residual content of ⁇ 1 wt.% NMMO washed and dried. The tendency to fibrillation of the fiber thus treated the grade 2 - 3.
  • the thread speed and the length of the blowing section is set so that the dwell time of the thread in the hot air zone is 3 ⁇ 1 Seconds results.
  • the tendency to fibrillation of those treated in this way Fiber received a grade of 2-3.
  • a fiber that has left the precipitation bath with 55% by weight NMMO is treated in a bath with an aqueous PVP solution that Contains 1% by weight additive and has a temperature of 22 ⁇ 3 ° C. Then the fiber is drawn through a treatment bath, that contains an aqueous solution of 50 wt.% NMMO and Is 22 ⁇ 3 ° C warm. The fiber speed and the Dimensions of the PVP- and NMMO-containing bath become like this chosen that a contact time of about 3 ⁇ 1 seconds per bath results. Then the fibers are at 140 ⁇ 10 ° C blown into hot air. The length of the hot air section will be like this set that a fiber dwell time in the hot air zone of 3 ⁇ 1 seconds results. Eventually the fiber becomes more well known Washed to a residual content of ⁇ 1 wt% NMMO and dried. The tendency to fibrillation of those treated in this way Fiber received a grade of 2-3.
  • NMMO / cellulose solution felling, washing and drying fiber obtained is through a treatment bath drawn, which has a temperature of 20 to 25 ° C.
  • Treatment bath is an aqueous solution of 47.6 wt% NMMO and 5.0 wt% PVP.
  • the fiber speed and the dimensions of the treatment bath are adjusted so that a fiber residence time of about 3 ⁇ 1 seconds results.
  • the fibers are blown with 140 ⁇ 10 ° C hot air.
  • the length of the hot air section is set so that a fiber dwell time in the hot air zone of 3 ⁇ 1 seconds results.
  • the fiber is made in a known manner a residual content of ⁇ 1 wt.% NMMO washed and dried. The tendency to fibrillation of the fiber thus treated received the marks 3 - 4.
  • One by spinning an NMMO / cellulose solution, felling, washing and drying fiber obtained is through a treatment bath drawn, which has a temperature of 65 ⁇ 5 ° C.
  • a treatment bath drawn in the treatment bath there is an aqueous solution of 65% by weight NMMO.
  • the fiber speed and the dimensions of the treatment bath are set so that a fiber residence time of about 4 seconds results.
  • the fibers passed through a bath filled with 120 ° C hot hexanol.
  • the length of the hexanol bath is adjusted so that a fiber residence time results in the bath of 5 ⁇ 1 seconds.
  • the fiber in a known manner to a residual content of ⁇ 1% by weight NMMO washed and dried.
  • the tendency to fibrillation of the Fiber treated in this way received a rating of 3-4.
  • One by spinning an NMMO / cellulose solution, felling, washing and drying obtained fiber is through a treatment bath drawn, which has a temperature of 80 ° C.
  • a treatment bath drawn which has a temperature of 80 ° C.
  • the breathing bath drawn which has a temperature of 80 ° C.
  • the treatment bath there is an aqueous solution of 70% by weight NMMO.
  • the fiber speed and the dimensions of the treatment bath are set so that a fiber residence time of about 2 seconds results.
  • the fiber in known Washed to a residual content of ⁇ 1 wt% NMMO and dried. The tendency to fibrillation of those treated in this way Fiber received the grade 3-4.
  • One by spinning an NMMO / cellulose solution, felling, washing and drying fiber obtained is through a treatment bath drawn, which has a temperature of 90 ° C.
  • a treatment bath drawn which has a temperature of 90 ° C.
  • the treatment bath there is an aqueous solution of 60% by weight NMMO and 2 wt% PVP.
  • the fiber speed and the dimensions of the treatment bath are set so that a fiber residence time of about 3 seconds results.
  • the Fiber in a known manner to a residual content of ⁇ 1% by weight NMMO washed and dried.
  • the tendency to fibrillation of the Fiber treated in this way received a rating of 3-4.
  • a fabric made of fibers made by spinning an NMMO / cellulose solution, Cases, washing and drying were made is treated as in Example 11. Then the tissue washed in a known manner to a residual content of ⁇ 1 wt.% NMMO and dried. The tendency of fibers to fibrillate, obtained from the tissue treated in this way the marks 3 - 4.

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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)
  • Artificial Filaments (AREA)
EP97915374A 1996-03-23 1997-03-17 Verfahren zur herstellung von cellulosischen fasern mit verringerter fibrillierungsneigung Expired - Lifetime EP0888467B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19611493 1996-03-23
DE19611493 1996-03-23
PCT/EP1997/001322 WO1997036028A1 (de) 1996-03-23 1997-03-17 Verfahren zur herstellung von cellulosischen fasern mit verringerter fibrillierungsneigung

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EP0888467A1 EP0888467A1 (de) 1999-01-07
EP0888467B1 true EP0888467B1 (de) 2000-02-02

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JP (1) JP2000507314A (id)
AT (1) ATE189487T1 (id)
AU (1) AU2288197A (id)
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ID (1) ID16295A (id)
TW (1) TW339367B (id)
WO (1) WO1997036028A1 (id)

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JP5421291B2 (ja) * 2008-01-16 2014-02-19 レンツィング アクチェンゲゼルシャフト 繊維混合物、それから製造された糸および織物
TWI667378B (zh) 2014-01-03 2019-08-01 奧地利商蘭精股份有限公司 纖維素纖維

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AT395724B (de) * 1990-12-07 1993-02-25 Chemiefaser Lenzing Ag Verfahren zur herstellung von celluloseformkoerpern
JPH07189125A (ja) * 1993-12-22 1995-07-25 Unitika Ltd セルロース繊維の加工方法
JPH07305218A (ja) * 1994-05-09 1995-11-21 Asahi Chem Ind Co Ltd 再生セルロースフイラメント糸の湿式処理方法
JP3445865B2 (ja) * 1995-04-06 2003-09-08 花王株式会社 セルロース系繊維改質法

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AU2288197A (en) 1997-10-17
TW339367B (en) 1998-09-01
EP0888467A1 (de) 1999-01-07
JP2000507314A (ja) 2000-06-13
WO1997036028A1 (de) 1997-10-02
ATE189487T1 (de) 2000-02-15
ID16295A (id) 1997-09-18

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