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Oxidative stabilisation of kraft lignin for carbon fibre production
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Wood Chemistry and Pulp Technology.
YKI.
Innventia.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Wood Chemistry and Pulp Technology.
2012 (English)In: Holzforschung, ISSN 0018-3830, Vol. 66, 141-147 p.Article in journal (Refereed) Published
Abstract [en]

With the aim of investigating kraft lignin as a raw material for carbon fibre production, different lignins have been stabilised in air at conditions varied according to a full factorial experimental design. The lignins under examination were purified kraft lignin powders originating from birch, spruce/pine and Eucalyptus globules, as well as lignin fibres originating from birch with 5% poly(ethylene oxide) (PEO) added as a plasticiser. The influence of temperature, time and heating rate on yield and glass-transition temperature (Tg) was investigated. The highest yield was achieved after stabilisation at 280C during 2 h with a heating rate of 0.2C min-1. The Tg of all lignin powders was increased when stabilisation occurred under harsher conditions. X-ray photoelectron spectroscopy analysis (XPS) of both the outer surface and the cleaved cross-section of individual lignin/PEO fibres showed a clear gradient in the degree of chemical modification, with the major change occurring on the surface resulting in the appearance of a skin-core structure after stabilisation. The behaviour of the lignin fibres during stabilisation is similar to that of pitch-based fibres, indicating good possibilities for lignin as raw material for carbon fibre production.

Place, publisher, year, edition, pages
Walter de Gruyter, 2012. Vol. 66, 141-147 p.
Keyword [en]
carbon fibre, differential scanning calorimetry, experimental design, kraft lignin, lignin fibre, stabilisation, X-ray photoelectron spectroscopy
National Category
Engineering and Technology
Identifiers
URN: urn:nbn:se:kth:diva-92252DOI: 10.1515/HF.2011.133ISI: 000300740500001OAI: oai:DiVA.org:kth-92252DiVA: diva2:513020
Funder
Knut and Alice Wallenberg Foundation
Note
QC 20120330Available from: 2012-03-30 Created: 2012-03-30 Last updated: 2012-03-30Bibliographically approved
In thesis
1. Carbon Fibres from Kraft Lignin
Open this publication in new window or tab >>Carbon Fibres from Kraft Lignin
2012 (English)Doctoral thesis, comprehensive summary (Other academic)
Alternative title[sv]
Kolfiber från sulfatlignin
Abstract [en]

Kraft lignin has a high potential for use in more valuable applications than its current use as fuel in pulp mills and integrated pulp and paper mills. The possibility of using kraft lignin, a green material with a carbon content of more than 60 %, for the manufacturing of carbon fibres was investigated in this thesis. The strong and lightweight carbon fibre material has many potential application areas, e.g. in cars; the main obstacle limiting its demand is the high production cost, with the raw material (petroleum pitch and polyactrylonitrile) and fibre spinning constituting approximately 50 % of the cost.

Industrial kraft lignins originating from both softwood (spruce/pine) and hardwood (birch/aspen) were isolated with the LignoBoost technique and then purified and characterized to determine the best suitable lignin for the production of carbon fibre. Using ultrafiltration of the black liquor before isolation using the LignoBoost technique, a kraft lignin with satisfactory high purity was obtained. The fractionated kraft lignin can be used either as such or as a softening agent during melt spinning to obtain continuously spun kraft lignin fibres.

The behaviour during thermal treatment was found to differ depending on the type of kraft lignin used. After oxidative stabilisation, the studied lignins became more stable, and thus, the final yield after carbonisation was increased by 10-20 % in comparison to stabilisation in absence of oxygen. The identified products indicate that the main reactions during oxidative stabilisation are radical, oxidation, condensation and rearrangement reactions.

The structural differences between softwood and hardwood kraft lignins facilitated the stabilisation of the softwood lignin fibre as compared with the hardwood lignin fibres. Thermal stabilisation in an inert atmosphere using only heat was successfully achieved for the softwood kraft lignin fibres. Stabilisation and carbonisation was successfully performed in a one-step operation on softwood kraft lignin fibres. Thus, it seems possible that the separate stabilisation step can be omitted, which may reduce the processing costs of softwood kraft lignin-based carbon fibres.

Abstract [sv]

Sulfatlignin har hög potential för att kunna användas i mer värdefulla applikationer jämfört med idag då det främst används som bränsle i massabruk och integrerade massa/pappersbruk. I egenskap av ett grönt material med en kolhalt på mer än 60 %, har möjligheterna att använda kraftlignin vid kolfibertillverkning undersöks i den här avhandlingen. Kolfiber är lätt och starkt med många olika potentiella användningsområden. Det som idag huvudsakligen begränsar efterfrågan är den höga produktionskostnaden, där råmaterialet (petroleum pitch och polyakrylonitril) och fiberspinningen står för ca 50 % av kostnaden.

Industriella sulfatligniner från både barrved (gran/tall) och lövved (björk/asp) har framställts enligt LignoBoost-processen och har därefter renats och karaktäriserats med syfte att hitta det mest lämpliga råmaterialet för tillverkning av kolfiber. Genom att använda ultrafiltrering av svartlut innan isolering med LignoBoost-tekniken, kan man få ett kraftlignin som är tillräckligt rent. Det fraktionerade kraftligninet kan användas antingen rent eller som mjukgörare under smältspinning, för att få fram kontinuerligt spunna sulfatligninfibrer.

Sulfatligniner från olika vedslag beter sig olika under termisk behandling. Efter oxidativ stabilisering blir ligninerna mer stabila jämfört med stabilisering i frånvaro av syre, vilket medför ett högre utbyte med 10-20 % av den slutgiltiga kolfibern efter karbonisering. De viktigaste reaktionerna som sker under oxidativ stabilisering av fibrer från sulfatlignin är radikal-, oxiderings- och omlagringsreaktioner.

De strukturella skillnaderna mellan sulfatlignin från barrved och lövved gör det möjligt att stabilisera barrvedslignin mycket fortare. Termisk stabilisering i inert atmosfär med endast värme har lyckats med sulfatligninfibrer från barrved. Vidare har även stabilisering och karbonisering i ett enda steg lyckats med sulfatligninfibrer från barrved. Detta kan göra det möjligt att utesluta stabiliseringssteget, vilket förhoppningsvis kan reducera processkostnaderna för kolfiber från barrvedssulfatlignin.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2012. xvii, 52 p.
Series
Trita-CHE-Report, ISSN 1654-1081 ; 2012:13
National Category
Engineering and Technology
Identifiers
urn:nbn:se:kth:diva-92256 (URN)978-91-7501-283-4 (ISBN)
Public defence
2012-04-20, STFI-salen, Drottning Kristinas väg 61, KTH, Stockholm, 10:00 (English)
Opponent
Supervisors
Note
QC 20120330Available from: 2012-03-30 Created: 2012-03-30 Last updated: 2012-03-30Bibliographically approved

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