WO2020254209A1 - Précurseur en lignine et procédé de fabrication d'un précurseur à partir de lignine pour la fabrication de fibres de carbone - Google Patents

Précurseur en lignine et procédé de fabrication d'un précurseur à partir de lignine pour la fabrication de fibres de carbone Download PDF

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Publication number
WO2020254209A1
WO2020254209A1 PCT/EP2020/066358 EP2020066358W WO2020254209A1 WO 2020254209 A1 WO2020254209 A1 WO 2020254209A1 EP 2020066358 W EP2020066358 W EP 2020066358W WO 2020254209 A1 WO2020254209 A1 WO 2020254209A1
Authority
WO
WIPO (PCT)
Prior art keywords
lignin
precursor
polymer
pas
yarn
Prior art date
Application number
PCT/EP2020/066358
Other languages
German (de)
English (en)
Inventor
Lars BOSTAN
Renate Fourné
Original Assignee
Faserinstitut Bremen E.V.
Fourné Maschinenbau Gmbh
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Faserinstitut Bremen E.V., Fourné Maschinenbau Gmbh filed Critical Faserinstitut Bremen E.V.
Publication of WO2020254209A1 publication Critical patent/WO2020254209A1/fr

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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
    • 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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins

Definitions

  • the invention relates to a method for producing a precursor from lignin according to the preamble of claim 1. Furthermore, the invention relates to a precursor from lignin according to claim 13.
  • the lignin used here is a bio-based raw material for the production of carbon fibers.
  • the lignin is used as a precursor material for the carbon fibers. Its molecular structure is similar to the widely used precursor material polyacrylonitrile (PAN).
  • PAN polyacrylonitrile
  • One of the outstanding properties of lignin is its melt spinnability. Because it is a by-product of paper production, it is also available in large quantities.
  • the invention is based on the object of creating a precursor made from lignin and a method with which carbon fibers can be produced from lignin.
  • a method for solving this problem has the measures of claim 1. Accordingly, it is provided that, in an extruder-based spinning process, lignin is pressed through at least one nozzle and encased by a polymeric jacket layer, in particular a thermoplastic jacket layer. This makes it possible to produce a lignin precursor yarn with greater than or equal to 1000 filaments and to process them further. Thanks to the protective polymer jacket layer, the yarn can be pinned several times in order to obtain the desired number of filaments. The subsequent modified conversion enables the production of endless, lignin-based carbon fibers or carbon fiber rovings with a sufficient number of filaments for industrial use.
  • the polymeric coating layer of the lignin is dissolved either in a solvent or in water, the coating layer preferably being formed from a water-soluble polymer.
  • the type of solvent for dissolving the jacket layer depends on the polymer used is selected. Depending on the type of polymer, it is conceivable to choose the solvent accordingly in order to bring about a particularly preferred detachment of the coat layer from the lignin.
  • lignin is melted and is pressed through at least one nozzle, so that the precursor is preferably composed of at least almost 100% lignin.
  • a spin carrier system with the water-soluble spin carrier in the island-in-the-sea spinning process is preferably used.
  • a core-sheath spinning process can also be used as a technical alternative. The subsequent conversion and storage makes it possible to create an endless, lignin-based carbon fiber roving with a sufficient number of filaments for industrial use.
  • the lignin and the polymer are pressed through the at least one nozzle at a temperature of 130 ° C. to 250 ° C., in particular from 160 ° C. to 220 ° C., preferably from 170 ° C. to 190 ° C.
  • This choice of material temperature allows the lignin to be processed particularly advantageously together with the polymer.
  • Preferred viscosities of the lignin and / or the polymer are 10 Pas to 2000 Pas, preferably 100 Pas to 2000 Pas, in particular 100 Pas to 500 Pas.
  • a particularly preferred viscosity ratio between the lignin and the polymer is 0.5 to 2.0. Due to this viscosity ratio, the polymeric sheath material can be joined particularly well around the lignin filaments in the process mentioned.
  • a multifilament yarn can be spun.
  • a carbon fiber with a multiple number of the named filaments can be produced.
  • the same is passed through the washing bath or a water bath in order to separate the polymer from the lignin.
  • This spinning process of the lignin with the polymeric coating layer and the subsequent washing bath provides a lignin precursor of up to 100%.
  • the unwinding of the yarn bobbins in the feed for stabilization is also made considerably easier by the carrier, since the carrier or the sheathing minimizes capillary breaks in the yarn during unwinding.
  • the at least almost pure lignin precursor can be stabilized by the temperature-controlled heating process, the precursor preferably being dried before stabilization. After the precursor has stabilized, the number of multifilaments for industrial use can be increased further by panning.
  • a stabilized continuous lignin yarn is either wound onto tubes, preferably bobbins, or is deposited in cans or is transported further to a subsequent carbonization process. After winding the lignin yarn onto a tube, it is possible to further ply several stabilized strands of lignin yarn.
  • a precursor for solving this problem has the features of claim 13. Accordingly, it is provided that a precursor consists of up to 100% lignin and can be fused together to form a yarn consisting of a large number of endless filaments.
  • the precursor can be produced by a method according to one of Claims 1 to 12.
  • a device 10 for the method according to the invention for producing a precursor 11 from lignin is illustrated by way of example in the single FIGURE of the drawing. It should be expressly pointed out that this device 10 is only one of many possible exemplary embodiments for producing the precursor 11 from lignin for carbon fibers. In addition to the device shown in the figure, it is conceivable that this device further or has fewer components with which the lignin precursor 11 is processed.
  • the lignin with the polymer After the lignin with the polymer has been processed into the lignin precursor yarn 11 in the melt spinning process under the conditions described above, it is placed on a spool 12, preferably on a plurality of spools 12, of a creel 13. Starting from this creel 13, several precursor yarns 11, which are each wound on different bobbins 12 of the creel 13, are brought together to ply. The multiply plied lignin precursor yarns 11 are then passed through a washing bath 14. In this washing bath 14, the polymeric jacket layer, which is preferably a thermoplastic, is separated from the lignin by a solvent, in particular water.
  • a solvent in particular water.
  • the plied yarn or multifilament is passed through a drying oven 15 in order to remove residual solvent or water from the filaments.
  • This preparation roller 16 is used to prepare or modify the multifilament accordingly before it enters the stabilization or oxidation oven 17.
  • This preparation roller 16 in particular protects the surface of the multifilaments or the yarn so that it can be easily transported in the post-treatment steps.
  • the necessary temperature is set by an air heater 18 in the furnace 17 depending on the material used.
  • the multifilaments are guided along several godets 19 in the oven 17 and converted. These godets 19 can be driven in such a way that they pull the filaments through the furnace.
  • the multifilaments are at least slightly stretched by slightly varying the rotational speeds of the godets 19 or by different rotational speeds of the godets 19.
  • the stabilization is achieved by the Heat application under oxygen in the furnace 17 carried out. After the stabilized filaments have left the furnace 17, they can either be deposited in a can or wound up by a winder 20 as shown in the figure. The yarn wound in this way can be transported on for a subsequent carbonization process or can be plied again in order to further increase the number of filaments in the yarn.
  • This process of melt spinning the lignin together with the polymer, separating the lignin from the jacket layer and then stabilizing the precursor in the furnace 17 with subsequent carbonization makes it possible to produce a carbon fiber yarn (roving) with a large number of filaments for industrial use to manufacture.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Inorganic Fibers (AREA)

Abstract

La lignine est une matière première biologique pour la fabrication de fibres de carbone. Mais jusqu'à maintenant aucun procédé n'est connu, au moyen duquel la lignine peut être transformée en fibres de carbone comprenant une pluralité de filaments pour l'application industrielle. L'invention concerne un précurseur (11) obtenu à partir de lignine et un procédé, au moyen duquel des fibres de carbone peuvent être fabriquées à partir de lignine. À cet effet, dans un procédé de filage basé sur une extrudeuse, la lignine est pressée à travers une buse et enveloppée d'une couche de revêtement polymère.
PCT/EP2020/066358 2019-06-17 2020-06-12 Précurseur en lignine et procédé de fabrication d'un précurseur à partir de lignine pour la fabrication de fibres de carbone WO2020254209A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102019004219.0A DE102019004219A1 (de) 2019-06-17 2019-06-17 Precursor aus Lignin und Verfahren zur Herstellung eines Precursors aus Lignin für die Herstellung von Kohlenstofffasern
DE102019004219.0 2019-06-17

Publications (1)

Publication Number Publication Date
WO2020254209A1 true WO2020254209A1 (fr) 2020-12-24

Family

ID=71096703

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2020/066358 WO2020254209A1 (fr) 2019-06-17 2020-06-12 Précurseur en lignine et procédé de fabrication d'un précurseur à partir de lignine pour la fabrication de fibres de carbone

Country Status (2)

Country Link
DE (1) DE102019004219A1 (fr)
WO (1) WO2020254209A1 (fr)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104593902A (zh) * 2015-02-15 2015-05-06 东华大学 一种碳纤维前驱体聚丙烯腈/木质素纤维的制备方法
WO2018138450A1 (fr) * 2017-01-27 2018-08-02 Institut De Recherche Technologique Jules Verne Procédé et formulation pour la préparation de fibres de lignine
US20190032250A1 (en) * 2016-01-26 2019-01-31 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e. V. Wet spinning method for producing a lignin-containing fiber as a precursor for a carbon fiber

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BR112013009692B1 (pt) * 2010-10-20 2020-09-29 Fitesa Germany Gmbh Tecido não tecido, tecido laminado, produto de tecido não tecido, fibra com múltiplos componentes, manta, e método para produzir o tecido não tecido
US10612163B2 (en) * 2017-08-24 2020-04-07 GM Global Technology Operations LLC Modification of continuous carbon fibers during precursor formation for composites having enhanced moldability

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104593902A (zh) * 2015-02-15 2015-05-06 东华大学 一种碳纤维前驱体聚丙烯腈/木质素纤维的制备方法
US20190032250A1 (en) * 2016-01-26 2019-01-31 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e. V. Wet spinning method for producing a lignin-containing fiber as a precursor for a carbon fiber
WO2018138450A1 (fr) * 2017-01-27 2018-08-02 Institut De Recherche Technologique Jules Verne Procédé et formulation pour la préparation de fibres de lignine

Also Published As

Publication number Publication date
DE102019004219A1 (de) 2020-12-17

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