EP2889401B1 - Regenerierte Cellulosefaser - Google Patents

Regenerierte Cellulosefaser Download PDF

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Publication number
EP2889401B1
EP2889401B1 EP13199757.9A EP13199757A EP2889401B1 EP 2889401 B1 EP2889401 B1 EP 2889401B1 EP 13199757 A EP13199757 A EP 13199757A EP 2889401 B1 EP2889401 B1 EP 2889401B1
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EP
European Patent Office
Prior art keywords
lignin
fiber
fibers
organosolv
cellulose fibre
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
EP13199757.9A
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German (de)
English (en)
French (fr)
Other versions
EP2889401A1 (de
EP2889401B2 (de
Inventor
Haio Harms
Daniela Bauer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Stora Enso Oyj
Original Assignee
Kelheim Fibres GmbH
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Publication date
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Application filed by Kelheim Fibres GmbH filed Critical Kelheim Fibres GmbH
Priority to EP13199757.9A priority Critical patent/EP2889401B2/de
Publication of EP2889401A1 publication Critical patent/EP2889401A1/de
Application granted granted Critical
Publication of EP2889401B1 publication Critical patent/EP2889401B1/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
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
    • D01F9/17—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate from lignin
    • 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
    • D01F2/08—Composition of the spinning solution or the bath
    • 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
    • D01F2/08—Composition of the spinning solution or the bath
    • D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either

Definitions

  • the present invention relates to a regenerated cellulose fiber produced by the viscose process (hereinafter also referred to as “viscose fiber”), to the production and use thereof.
  • the present invention relates to a regenerated cellulosic fiber containing lignin.
  • Viscose fibers are already used in carbonized insulating moldings and nonwovens.
  • carbonaceous starting materials precursors
  • precursors are pyrolyzed in an oven at temperatures of 500-1800 ° C with exclusion of oxygen.
  • This foreign atoms such as nitrogen, oxygen and hydrogen are split off in gaseous form.
  • What remains is almost exclusively carbon, which has a graphite-like layer structure.
  • the carbonation yield of viscose is theoretically 44%, but in reality only 15-20%. Thus, 80 to 85% of the fiber mass is lost during the carbonization. By improving the carbon yield, the carbonation process would be much more economical.
  • the WO 2012/156443 A1 describes precursor fibers for producing carbon fibers containing lignin.
  • the fibers are spun from a solution containing a lignin and a fiber-forming polymer from the group of polyacrylonitrile or polyacrylonitrile copolymers.
  • Example 2 of this document describes the spinning of a solution containing chemical cellulose, kraft lignin and polyacrylonitrile.
  • the WO 2013/020919 deals with the production of precursor fibers from carbon fibers.
  • the fiber is a mixture of polyacrylonitrile, a glucan and lignin. Both in the case of WO 2012/156443 A1 as well as the WO 2013/020919
  • the fibers are spun from a solution in an organic solvent.
  • the EP 2 524 980 describes the production of precursor fibers from carbon fibers.
  • the fibers contain at least 10% lignin and one or more fiber-forming polymers, such as cellulose, and are spun from an organic solvent.
  • the object underlying the present invention is achieved by a regenerated cellulose fiber containing Organosolv lignin.
  • the most important pulping processes are the sulphate process (product: kraft lignin) and the sulphite process (product: lignosulphonates). More than 50 million tonnes of lignin are isolated as a by-product every year.
  • the lignins differ in their monomer composition, type of bonds and their molecular weight depending on the plant species, origin and season. In addition, each digestion process produces lignins with other properties.
  • Organosolv lignin By the "Organosolv method" the skilled person understands a wood pulping with the aid of aqueous organic solvents, in particular ethanol, at high pressure and high temperature.
  • aqueous organic solvents in particular ethanol
  • the resulting lignin in this process is called Organosolv lignin.
  • the cellulose fiber of the invention may have a content of Organosolv lignin of 5% to 90%, preferably 10% to 70%, particularly preferably 20% to 50%, based on fiber.
  • Organosolv lignin 5% to 90%, preferably 10% to 70%, particularly preferably 20% to 50%, based on fiber.
  • (regenerated) cellulosic fiber” or “viscose fiber” shall also include fibers containing up to 90% lignin, as long as it is by the viscose process, ie from an alkaline solution containing cellulose xanthate and spun into an acid spin bath , getting produced.
  • the fiber of the invention may preferably contain another lignin different from organosolv lignin. Because organosolv lignin is less soluble than common lignins, e.g. Kraft-lignin or lignosulfonates is more difficult to obtain, by replacing a portion of the Organosolv lignin by another lignin production of the fiber of the invention and the carbon fiber resulting therefrom carbonization can be made even more favorable.
  • organosolv lignin is less soluble than common lignins, e.g. Kraft-lignin or lignosulfonates is more difficult to obtain, by replacing a portion of the Organosolv lignin by another lignin production of the fiber of the invention and the carbon fiber resulting therefrom carbonization can be made even more favorable.
  • the further lignin is preferably selected from the group consisting of kraft lignin, lignosulfonate and mixtures thereof.
  • the further lignin is preferably uncrosslinked.
  • the content of further lignin in the fiber may be from 5% to 85%, preferably from 10% to 70%, particularly preferably from 20% to 50%, based on fiber.
  • the ratio of organosolv lignin to further lignin may be from 4: 1 to 1: 4, preferably 3: 1 to 1: 3.
  • the cellulosic fiber of the present invention is characterized by substantially no further fiber-forming polymer, such as cellulose and lignin. Polyacrylonitrile or polyacrylonitrile copolymers containing.
  • the cellulose fiber according to the invention may have a titer of 0.5 dtex to 30 dtex, preferably 1 dtex to 4 dtex.
  • the cellulose fiber according to the invention is preferably used for the production of carbon fibers. Further fields of use are e.g. Hygiene and medical applications (due to the increased water retention capacity of the fiber).
  • the present invention also relates to a process for producing the cellulosic fiber of the invention, comprising the step of adding organosolv lignin and optionally another lignin to a spun viscose or a precursor thereof.
  • precursors of a spinning viscose are in particular starting substances of the viscose process, such as e.g. Pulp, or intermediates such as e.g. Alkali cellulose or cellulose xanthogenate understood.
  • the lignin was mixed in a proportion of 50% based on the total amount of fiber-forming polymer (cellulose + lignin) in a standard viscose.
  • the lignin was when spinning each in the form of a solution with 30% lignin in 5% NaOH before.
  • the lignin-containing viscoses were spun according to standard conditions.
  • the target denier of the fibers was 3.3 dtex, the draw was 25%.
  • the resulting fibers were washed out in a conventional manner.
  • the lignin contents in the finished fiber were first on the Klason Method (Tappi Test Methods 2001-2002, T 222 om-02 Tappi Press ). According to this method, the acid-insoluble lignin ("Klason lignin”) is detected gravimetrically. In addition, the acid-soluble lignin is determined photometrically (Tappi UM 250, wavelength: 205 nm, absorption coefficient: 110 L / (g.cm)). The photometric determination using these parameters is the usual method in the art, although it is known that the results obtained with respect to the different lignin types can vary slightly. For the purposes of the present invention, it is thus defined that the determination of the acid-soluble lignin content must be made using these parameters.
  • the lignosulfonate is thus washed out due to the very good solubility already during the spinning of the fiber and in the subsequent wash to a large extent. Only 11% lignin (absolute) was found in the fiber, so 77% of the lignin offered was washed out. Organosolv lignin shows the highest retention. The fiber contains 38% lignin, while 23% of the offered lignin was washed out. A medium retention shows the force lignin with a content of absolutely 27% lignin in the fiber, while 45% (relatively) were washed out.
  • the fiber had a titer of 3.24 dtex.
  • the maximum tensile force in cN was 6.71, the elongation 18.79%.
  • the fiber had a denier of 3.66 dtex.
  • the maximum tensile force in cN was 5.72, the elongation 17.95%.
  • Example 2 Analogously to Example 1, a mixture of 35% uncrosslinked Organsolv lignin of the type batch K002 (manufacturer: Fraunhofer Institute CBP) and 15% of the lignosulfonate used in Example 1, in each case based on the total amount of fiber-forming polymer (cellulose + lignin), a viscose blended and the resulting solution spun into fibers.
  • the mixture showed very good spinning stability.
  • the fiber had a titer of 2.72 dtex.
  • the maximum tensile force in cN was 2.78, the elongation 17.12%.
  • the water retention was 123%.
  • the fibers are distinguished by a dark brown color.
  • the fibers prepared according to Example 1 with (nominal) 50% addition of lignin show a very smooth surface with mainly C-shaped cross-sections. These cross sections are in the FIG. 1 shown.
  • lignin-containing fibers show a significantly higher absorption (higher water retention capacity) compared to a normal viscose fiber, making them ideal for use in hygiene products.
  • the (inter alia) containing lignosulfonate fiber according to Example 4 contains sulfonic acid groups which act as ion exchangers.
  • organosolv lignin or a mixture of organosolv lignin and lignosulfonate-containing viscose fibers prepared according to Examples 1, 2 and 4 were carbonized (Gero oven, 20 ° C. to 1800 ° C., heating rate 10 K / min under a nitrogen atmosphere). The carbon yield was compared to that of a standard viscose fiber.

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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)
  • Inorganic Fibers (AREA)
EP13199757.9A 2013-12-30 2013-12-30 Regenerierte Cellulosefaser Active EP2889401B2 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP13199757.9A EP2889401B2 (de) 2013-12-30 2013-12-30 Regenerierte Cellulosefaser

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP13199757.9A EP2889401B2 (de) 2013-12-30 2013-12-30 Regenerierte Cellulosefaser

Publications (3)

Publication Number Publication Date
EP2889401A1 EP2889401A1 (de) 2015-07-01
EP2889401B1 true EP2889401B1 (de) 2016-02-24
EP2889401B2 EP2889401B2 (de) 2020-04-29

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ID=49882952

Family Applications (1)

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EP13199757.9A Active EP2889401B2 (de) 2013-12-30 2013-12-30 Regenerierte Cellulosefaser

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EP (1) EP2889401B2 (tr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106149081B (zh) * 2015-04-02 2019-05-17 河北吉藁化纤有限责任公司 一种再生纤维素纤维制备方法及其纤维
WO2025158263A1 (en) * 2024-01-22 2025-07-31 Stora Enso Oyj Method for producing a carbon fiber precursor from lignin and cellulose xanthate as well as a carbon fiber precursor

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012156441A1 (en) 2011-05-18 2012-11-22 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method for the production of lignin-containing precursor fibres and also carbon fibres
WO2014162062A1 (en) 2013-04-04 2014-10-09 Aalto University Foundation Process for the production of shaped cellulose articles

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4215212A (en) * 1979-04-09 1980-07-29 Akzona Incorporated Regenerated cellulose containing cross linked sodium lignate or sodium lignosulfonate
JP2002105746A (ja) * 2000-09-29 2002-04-10 Araco Corp 改質アセテート繊維およびその製造方法、繊維積層体成形品およびその製造方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012156441A1 (en) 2011-05-18 2012-11-22 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method for the production of lignin-containing precursor fibres and also carbon fibres
WO2014162062A1 (en) 2013-04-04 2014-10-09 Aalto University Foundation Process for the production of shaped cellulose articles

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EP2889401A1 (de) 2015-07-01
EP2889401B2 (de) 2020-04-29

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