WO2019077208A1 - Procédé de fabrication de filaments de fil à base de bois - Google Patents

Procédé de fabrication de filaments de fil à base de bois Download PDF

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Publication number
WO2019077208A1
WO2019077208A1 PCT/FI2018/050770 FI2018050770W WO2019077208A1 WO 2019077208 A1 WO2019077208 A1 WO 2019077208A1 FI 2018050770 W FI2018050770 W FI 2018050770W WO 2019077208 A1 WO2019077208 A1 WO 2019077208A1
Authority
WO
WIPO (PCT)
Prior art keywords
des
solvent
cellulose
pulp
cellulosic material
Prior art date
Application number
PCT/FI2018/050770
Other languages
English (en)
Inventor
Hannes Orelma
Ali Harlin
Hille RAUTKOSKI
Ville KLAR
Original Assignee
Teknologian Tutkimuskeskus Vtt Oy
Aalto-Korkeakoulusäätiö Sr
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 Teknologian Tutkimuskeskus Vtt Oy, Aalto-Korkeakoulusäätiö Sr filed Critical Teknologian Tutkimuskeskus Vtt Oy
Priority to EP18804034.9A priority Critical patent/EP3697950A1/fr
Publication of WO2019077208A1 publication Critical patent/WO2019077208A1/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
    • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/02—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet spinning methods
    • 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

Definitions

  • the present invention relates to a method for producing wood-based yarn filaments from DES-pulp suspension.
  • Cellulose plays an important role in textile and filament production.
  • the long fibers of natural cotton are ideal for forming strong filaments and yarns, whereby cotton is traditionally utilized in textiles.
  • the use of cotton requires lots of water, pesticides and fertilizers in the production phase.
  • Wood-based fabrics have been suggested as an ecologically friendly alternative for cotton.
  • wood-based cellulose is generally formed as a filament made of dissolved and regenerated cellulose.
  • This is also the process that the manmade cellulose-based textile fibres e.g. viscose, modal and lyocell are based on today.
  • harmful or toxic chemicals are used, which also have negative effect on the properties of cellulose.
  • most of the regenerated cellulose processes are considered unsustainable, and as the crystalline form of cellulose changes in the process, the material properties change drastically as well.
  • Short wood fibres do not naturally form strong filaments and they have a tendency to disintegrate in water.
  • Ionic solvents have been proposed for dissolving cellulosic materials originating from natural sources. However, they are often harmful or toxic and very expensive for industrial use on a larger scale.
  • Deep eutectic solvents are a type of ionic solvents which refer to eutectic mixtures, which melting points are lower than the individual components of separately. Deep eutectic solvents are currently applied in large scale applications, such as electro winning of metals, electro polishing of stainless steel, as well as solvents in organic reactions.
  • WO 2012/145522 relates to deep eutectic solvents for the purpose of dissolving cellulose.
  • DES-pulp is typically manufactured into the fibre yarn filament by extruding it into ethanol bath.
  • the function of the ethanol has been to dissolve the DES away, which requires long time, such as up to 15 minutes.
  • NFC fibre yarn filaments have a tendency to stick into the rollers/cylinders in the production process.
  • the fiber yarn filament according to an embodiment of the present invention is mainly characterized by what is stated in claim 9 and the use thereof by what is stated in claim 10.
  • the present invention provides a simple non-toxic method that uses DES-pulp and laminar solvent flow to produce strong and water- stable fiber yarn filaments.
  • the method enables producing more fibre yarn filaments in the same time span as currently has been possible.
  • the solvent can be circulated and used again during the production process.
  • the present invention reduces the investment costs and the production time and enables easier upscaling of the process.
  • the present technology describes a method for manufacturing DES-pulp suspension into a fibre yarn filament.
  • the method is continuous.
  • Deep eutectic solvents are a sub-class of ionic liquids with special properties. DES is composed of a mixture of two or more components and said mixture forms a eutectic with a melting point much lower than any of the individual components.
  • the deep eutectic solvent useful in the present invention consists of hydrogen bond donor and hydrogen bond acceptor.
  • FIGURE 1 is a process scheme describing one embodiment of the present invention.
  • FIGURE 2 is a process scheme describing another embodiment of the present invention.
  • the present invention is based on extruding DES-pulp suspension into flowing solvent.
  • the function of the flowing solvent is to dissolve DES from the extruded filament.
  • Laminar flow of the solvent immediately starts the dissolution process of DES, providing substantially shortened DES-removal time. In turn, this enables less time consuming method for yarn filament production from such starting material.
  • the deep eutectic solvent is selected from the group consisting of DESs, which are able to swell cellulosic material without dissolving it, whereby the cellulosic material can be dispersed in the DES.
  • the DESs suitable for the present invention are selected from DESs composed of choline chloride and urea, choline chloride and malonic acid, choline chloride and oxalic acid, choline chloride and phenylacetic acid, and choline chloride and glycerol.
  • Choline chloride acts as the hydrogen bond acceptor and the hydrogen bond donor is selected from urea, malonic acid, oxalic acid, phenylacetic acid and glycerol.
  • a DES composed of choline chloride and urea is used.
  • the DES comprises a molar ratio from 5: 1 to 1 :3, preferably from 3: 1 to 1 :2 of choline chloride and the hydrogen bond donor, respectively. Particularly preferably a molar ratio 1 :2 of choline chloride and the hydrogen bond donor, preferably urea is used. Suitable molar ratio for choline chloride and malonic acid is 1 : 1.
  • One embodiment of the present invention is a method for continuously producing wood-based yarn filaments, the method having at least the steps of: suspending a cellulosic material in a DES (deep eutectic solvent) comprising choline chloride and urea at temperature of 10 to 280 °C for obtaining a DES-pulp suspension, and extruding the DES-pulp suspension into a solvent, wherein the DES-pulp suspension is extruded into a running laminar solvent flow at a speed of 1 to 15 cm/s, after which the produced fiber yarn filaments are collected and dried.
  • DES deep eutectic solvent
  • the method uses a solvent which is an alcohol that is capable to dissolve the components of the used DES.
  • the solvent is ethanol.
  • suspending a cellulosic material in DES comprising choline chloride and urea is carried out at temperature of 10 to 130 °C for obtaining the desired DES-pulp suspension.
  • the laminar solvent flow speed is between 2 and 10 cm s, preferably between 3 and 6 cm/s, such as 4.5 cm/s. It is possible to change the solvent flow speed for example by altering the pumping speed or by changing the angle of the gutter, wherein the extrusion takes place.
  • the solvent is recycled back to the process by a pump and used at least two times.
  • the cellulosic material may comprise a wide variety of cellulose based raw materials. For example pulp fibres derived from wood pulp may be used.
  • mechanically treated pulp fibres such as chemithermomechanical pulp fibres (CTMP), bleached chemithermomechanical pulp fibres (BCTMP), thermomechanical pulp fibres (TMP), refiner groundwood pulp fibres, groundwood pulp fibres, enzymatically treated pulp, cellulose microparticles, cellulose nanoparticles, micro fibrillated cellulose, nanocellulose, enzymatically fibrillated cellulose, and combinations thereof may be used.
  • CMP chemithermomechanical pulp fibres
  • BCTMP bleached chemithermomechanical pulp fibres
  • TMP thermomechanical pulp fibres
  • refiner groundwood pulp fibres groundwood pulp fibres
  • groundwood pulp fibres enzymatically treated pulp
  • cellulose microparticles cellulose nanoparticles
  • micro fibrillated cellulose nanocellulose
  • enzymatically fibrillated cellulose and combinations thereof
  • the cellulosic material is hardwood pulp. This is preferred in order to obtain continuous fibre yarn filaments.
  • Thickness of the fiber yarn filament may be changed according to the end-use purpose by altering the nozzle size in the extrusion.
  • Single filaments with variable thickness can also be twisted and plied into multifilament yarns with texture depending on the plying technique. Twisting even a single filament improves tenacity values and plying and cabling several filaments improves the values even more.
  • Fibre yarn filaments from cellulosic materials is considered as a sustainable alternative for cotton.
  • the use of these alternative wood-based raw materials reduces sweet water consumption, particularly for irrigation, as well as occupation of agricultural land and the use of plant protection chemicals.
  • a further advantage of the present invention is the recyclability of the DES and solvents used in the process.
  • At least some embodiments of the present invention find industrial application among for example yarns, ropes, textiles and cloths.
  • the obtained filaments are stable in water.
  • the water stable filaments are used as such, but plying them into multifilament yarns and ropes further widens their use.
  • textile applications benefit from lightness and possibility for coloured or multicoloured yarn.
  • the obtained high quality wood cellulose filaments can be used in wood-based cellulosic fabrics. These fabrics can be used where ever natural fibre fabrics are needed, e.g. clothing, technical textiles etc., thus providing inexpensive and eco- friendly wood-based textiles.
  • the high quality wood cellulose filaments are particularly suitable for products which are directly dependent on long fibre filament.
  • the DES-pulp solution was prepared as follows. ChCl/urea DES was prepared by mixing ChCl and urea together in a mole ratio of 1 :2, respectively and heated at 100°C with constant stirring until a clear homogenous liquid was formed, followed by drying at 40°C overnight under vacuum, whereby the water content was reduced to less than 1 wt%. Prior to adding in ChCl/urea, the pulp was washed with excess acetone and dried at 40°C overnight under vacuum whereby the water content was reduced to less than 1 wt%. Spinning dopes were prepared by dispersing the pulp in ChCl/urea overnight at 100°C temperature with constant stirring. The dispersions were then cooled and mixed in a Speedmixer under vacuum (800 rpm for 2 min and 1500 rpm for 8 min).
  • the DES containing typically 4 % of anhydrous pulp fibres was place into a syringe containing a nozzle with required dimensions.
  • the DES-pulp suspension is extruded into a laminar ethanol flow in a canal with downward slope (5-20 degrees).
  • the ethanol flow takes the wet filament ribbon from the nozzle and transports the wet filament ribbon into the collection chamber.
  • the flow rate of ethanol is above the flow rate of the DES-pulp suspension from the nozzle.
  • the difference in the flowrate maintains straight filament direction and can stretch the filament.
  • the continuous flow around the filament accelerates the diffusion out of the DES chemicals from the filament.
  • the filament After keeping the filament in the collection chamber for 30 to 120 min, the filament is wound and heat activated in an oven at 130 °C for 20 min.

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)
  • Multicomponent Fibers (AREA)
  • Paper (AREA)

Abstract

Selon un aspect de la présente invention donné à titre d'exemple, l'invention concerne un procédé de production de filaments de fil à base de bois à partir de pâtes à base de solvant eutectique profond (DES) faisant appel à un système d'extrusion et d'écoulement laminaire de solvant.
PCT/FI2018/050770 2017-10-20 2018-10-22 Procédé de fabrication de filaments de fil à base de bois WO2019077208A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP18804034.9A EP3697950A1 (fr) 2017-10-20 2018-10-22 Procédé de fabrication de filaments de fil à base de bois

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI20175927A FI127726B (en) 2017-10-20 2017-10-20 Process for making wood-based yarn filaments
FI20175927 2017-10-20

Publications (1)

Publication Number Publication Date
WO2019077208A1 true WO2019077208A1 (fr) 2019-04-25

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/FI2018/050770 WO2019077208A1 (fr) 2017-10-20 2018-10-22 Procédé de fabrication de filaments de fil à base de bois

Country Status (3)

Country Link
EP (1) EP3697950A1 (fr)
FI (1) FI127726B (fr)
WO (1) WO2019077208A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111384462A (zh) * 2019-12-27 2020-07-07 中国矿业大学 一种从废旧锂离子电池负极材料中回收石墨制备石墨烯的方法
WO2021165572A1 (fr) * 2020-02-18 2021-08-26 Aalto University Foundation Sr Système de bain de coagulation pour filage de fibres
US11713528B2 (en) 2021-08-31 2023-08-01 Apani Systems Inc. Textile recycling
WO2023208257A1 (fr) * 2022-04-29 2023-11-02 齐鲁工业大学(山东省科学院) Procédé d'amélioration de structure de surface de fibre de cellulose régénérée

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012145522A2 (fr) 2011-04-19 2012-10-26 Georgia Tech Research Corporation Systèmes de solvant eutectique profond et procédés
WO2016135385A1 (fr) * 2015-02-27 2016-09-01 Teknologian Tutkimuskeskus Vtt Oy Procédé de production d'articles façonnés à base de cellulose

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012145522A2 (fr) 2011-04-19 2012-10-26 Georgia Tech Research Corporation Systèmes de solvant eutectique profond et procédés
WO2016135385A1 (fr) * 2015-02-27 2016-09-01 Teknologian Tutkimuskeskus Vtt Oy Procédé de production d'articles façonnés à base de cellulose

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
KARL M. O. HÅKANSSON ET AL: "Hydrodynamic alignment and assembly of nanofibrils resulting in strong cellulose filaments", NATURE COMMUNICATIONS, vol. 5, no. 1, 2 June 2014 (2014-06-02), XP055545700, DOI: 10.1038/ncomms5018 *
MERI J. LUNDAHL ET AL: "Spinning of Cellulose Nanofibrils into Filaments: A Review", INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH, vol. 56, no. 1, 2 December 2016 (2016-12-02), pages 8 - 19, XP055474988, ISSN: 0888-5885, DOI: 10.1021/acs.iecr.6b04010 *
TIIA-MARIA TENHUNEN ET AL: "Method for Forming Pulp Fibre Yarns Developed by a Design-driven Process", BIORESOURCES, 26 January 2016 (2016-01-26), pages 2492 - 2503, XP055545626, Retrieved from the Internet <URL:http://ojs.cnr.ncsu.edu/index.php/BioRes/article/view/8151> [retrieved on 20190122], DOI: 10.15376/biores.11.1.2492-2503 *
VILLE KLAR ET AL: "Spinning Approach for Cellulose Fiber Yarn Using a Deep Eutectic Solvent and an Inclined Channel", ACS OMEGA, vol. 3, no. 9, 10 September 2018 (2018-09-10), pages 10918 - 10926, XP055545636, ISSN: 2470-1343, DOI: 10.1021/acsomega.8b01458 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111384462A (zh) * 2019-12-27 2020-07-07 中国矿业大学 一种从废旧锂离子电池负极材料中回收石墨制备石墨烯的方法
WO2021165572A1 (fr) * 2020-02-18 2021-08-26 Aalto University Foundation Sr Système de bain de coagulation pour filage de fibres
US11713528B2 (en) 2021-08-31 2023-08-01 Apani Systems Inc. Textile recycling
WO2023208257A1 (fr) * 2022-04-29 2023-11-02 齐鲁工业大学(山东省科学院) Procédé d'amélioration de structure de surface de fibre de cellulose régénérée

Also Published As

Publication number Publication date
EP3697950A1 (fr) 2020-08-26
FI127726B (en) 2019-01-15
FI20175927A1 (fi) 2019-01-15

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