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This is an electronic reprint of the original article.This reprint may differ from the original in pagination and typographic detail.
Author(s): Hauru, Lauri; Hummel, Michael; Michud, Anne; Sixta, Herbert
Title: Dry jet-wet spinning of strong cellulose filaments from ionic liquidsolution
This publication is included in the electronic version of the article dissertation:Hauru, Lauri K.J. Lignocellulose solutions in ionic liquids.Aalto University publication series DOCTORAL DISSERTATIONS, 87/2017.
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Dry jet-wet spinning of strong cellulosefilaments from ionic liquid solution
Lauri K. J. Hauru, Michael Hummel, Anne Michud, Herbert Sixta
Department of Forest Products Technology, Aalto University, School of ChemicalEngineering, P.O. Box 16300, 00076 Aalto, Espoo, FinlandPhone: +358-50-384 1764
A dry-jet wet spinning process for spinning cellulose fibers from an ionic liquid
solution is characterized and its limitations and sensitivities discussed. A 13 wt-%
solution of dissolving pulp in an ionic liquid ([DBNH][OAc]) was extruded and
drawn in air and regenerated in water. With extrusion velocities in the range 0.02
to 0.04 ml min–1, drawing in the air gap with DR 7.5–12.5 gave filaments with
high tenacities (36.8±2.2 cN tex–1 or 552±34 MPa) and moduli (15.4±2.0 cN tex–1
%–1 or 23.2±3.1 GPa). Linear density of the finished fibers was proportional to
DR–1. This suggests a simple deformation, rather than the more complicated
deformation seen in NMMO spinning, where the viscosity increase in the air gap
due to cooling leads to a dependency on DR–0.5 instead (Kong and Eichhorn 2005).
Mechanical properties (tenacity, modulus, resilience) and birefringence were
independent of extrusion velocity, and orientation was nearly complete at DR 5.
The lack of a speed dependency suggests again a simple deformation, where
amorphous domains are stretched and thus oriented in lockstep with crystalline
regions. This is explicitly revealed by dry/wet modulus ratio changing from 9 to 4
with increasing draw ratio. Strong filaments were readily spun only with a
coagulation bath temperature of 15 °C, but not with 30 or 45 °C. A spinneret
aspect ratio (L/D) of 2.0 gave a better orientation than L/D 0.2 and allowed to
reach higher draw ratios. However, our small-scale monofilament setup seems to
slightly damage high-draw ratio filaments, because there is slipping on the takeup
godet. Thus, improvement is expected when spinning in multifilament mode,
where the fiber bundle is stronger and less likely to slip than a single filament. In
summary, the process was found to be robust and simple even with the suboptimal
setup of a small monofilament system, and in performance comparable to the
commercial NMMO-based Lyocell process.
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Acknowledgements The authors wish to thank TEKES – the Finnish Funding Agency for
Technology and Innovation and Finnish Bioeconomy Cluster FIBIC Ltd. for funding in the
framework of the Future Biorefinery Cellulose project. Arno Parviainen synthesized the
[DBNH][OAc] with Dr. Alistair King and Prof. Ilkka Kilpeläinen (University of Helsinki). Dope
samples were kindly provided by Shirin Asaadi. Kaarlo Nieminen assisted with MatLab and GPC
was operated by Lasse Tolonen.
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