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Sulfur-free dissolving pulps and their application for viscose and lyocell

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Abstract

In this study, the concept of multifunctional alkaline pulping has been approved to produce high-purity and high-yield dissolving pulps. The selective removal of hemicelluloses was achieved by either water autohydrolysis (PH) or alkaline extraction (E) both applied as pre-treatments prior to cooking. Alternatively, hemicelluloses were isolated after oxygen delignification in a process step denoted as cold caustic extraction (CCE). Eucalyptus globulus wood chips were used as the raw material for kraft and soda-AQ pulping. In all process modifications sulfur was successfully replaced by anthraquinone. By these modifications purified dissolving pulps were subjected to TCF bleaching and comprehensive viscose and lyocell application tests. All pulps met the specifications for dissolving pulps. Further more, CCE-pulps showed a significantly higher yield after final bleaching. Morphological changes such as ultrastructure of the preserved outer cell wall layers, specific surface area and lateral fibril aggregate dimension correlated with the reduced reactivity towards regular viscose processing. The residual xylan after alkali purification depicted a lower content of functional groups and a higher molecular weight and was obviously entrapped in the cellulose fibril aggregates which render the hemicelluloses more resistant to steeping in the standard viscose process. Simultaneously, the supramolecular structure of the cellulose is partly converted from cellulose I to cellulose II by the alkaline purification step which did not influence the pulps reactivity significantly. Nevertheless, these differences in pulp parameters did not affect the lyocell process due to the outstanding solubility of the pulps in NMMO. Laboratory spinning revealed good fiber strength for both, regular viscose and lyocell fibers. The high molecular weight xylan of the CCE-treated pulps even took part in fiber forming.

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Abbreviations

AEC:

Anion exchange chromatography

AH:

Acid hydrolysis

as,BET :

Specific surface area according to Brunauer, Emmett and Teller

AQ:

Anthraquinone

CBC:

Continuous batch cooking

CCE:

Cold caustic extraction

CRI:

Crystallinity index

DP:

Degree of polymerisation

E:

Alkaline pre-extraction

EA:

Effective alkali

FE-SEM:

Scanning electron microscope

HCE:

Hot caustic extraction

HexA:

Hexenuronic acid

K:

Kraft pulp

LFAD:

Lateral fibril aggregate dimension

MALLS:

Multi-angel laser light scattering

MWD:

Molecular weight distribution

Mw:

Molecular weight

n.d.:

Not determined

NMMO:

N-methyl-morpholine-N-oxid

O:

Oxygen-bleaching-stage

Odp:

Oven dry pulp

Odw:

Oven dry wood

P:

Hydrogenperoxide bleaching stage

PAD:

Pulsed amperometric detection

PDI:

Polydispersity index

PH:

Prehydrolysis

PW:

Primary cell wall

SAQ:

Soda-AQ pulp

SEC:

Size exclusion chromatography

S1:

Secondary cell wall 1

S2:

Secondary cell wall 2

TCF:

Total chlorine free

WRV:

Water retention value

Z:

Ozone bleaching stage

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Acknowledgments

Financial support was provided by the Austrian government, the provinces of Lower Austria, Upper Austria, and Carinthia as well as by the Lenzing AG. We also express our gratitude to the Johannes Kepler University, Linz, the University of Natural Resources and Applied Life Sciences, Vienna, and the Lenzing AG for their in-kind contributions.

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  1. Kompetenzzentrum Holz GmbH, St.-Peter-Str. 25, 4021, Linz, Austria

    Gabriele Schild

  2. Lenzing AG, Werkstraße 1, 4860, Lenzing, Austria

    Herbert Sixta

  3. Department of Forest Products Technology, Helsinki University of Technology, Vuorimiehentie 1, 02015, Espoo, Finland

    Herbert Sixta

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  1. Gabriele Schild
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  2. Herbert Sixta
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Correspondence to Gabriele Schild.

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Schild, G., Sixta, H. Sulfur-free dissolving pulps and their application for viscose and lyocell. Cellulose 18, 1113–1128 (2011). https://doi.org/10.1007/s10570-011-9532-0

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