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Reactive extrusion of cellulose fibes as feasible way to process value added products

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By Nikita Polikarpov, Papiertechnische Stiftung (PTS), This was presented during the New Ideas for the Paper Industry: Young Researchers' Presentations session, organised as part of European Paper Week 2015. More at http://www.cepi.org/epw

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Reactive extrusion of cellulose fibes as feasible way to process value added products

  1. 1. Reactive extrusion of cellulose fibres as a feasible way to process value added products Nikita Polikarpov Brüssel, 17.11.2015
  2. 2. 17.11.2015 Sustainable development in paper industry Paper industry is looking for • new markets • new products • new approaches Is it possible to imagine… • Cellulose as a source for bioplastics? • Cellulose fibres as reinforcement in composites? • Cellulose fibre as thermoplastic? Yes, but there are some issues… • Cellulose esters (bioplastic) are costly. • Poor interactions between hydrophilic cellulose fibres and hydrophobic thermoplastics. • Cellulose decomposes below its glass-transition temperature. 2
  3. 3. 17.11.2015 PTS Platform Technology Reactive Extrusion 3 Various monomers and reactive compounds Pulp Amorphous cellulose derivatives Surface modified pulp fibres (hydrophobic, thermoplastic) Surface modified microfibrillated cellulose • Thermoplastic paper based products • Reinforcement in composites / Light weight construction • Masterbatches • Injection moulding New markets / products New approach
  4. 4. 17.11.2015 Twin Screw Extruder 4 Source: Coperion Kneading element Tooth-mixing element Conveying element Modular design for screw elements and kneading blocks
  5. 5. 17.11.2015 EXAMPLE 1 CELLULOSE ACETYLATION 5
  6. 6. 17.11.2015 Cellulose Acetate 6 Dominant thermoplastic cellulose based product is cellulose acetate (~80,000 t/p.a.) • Properties depend on substitution degree DS and polymerisation degree DP DS Application 1.8–1.9 Composite fabrics 2.2–2.3 Lacquers, plastics 2.3–2.4 Acetate rayon 2.5–2.6 Safety films 2.8–2.9 Insulation foils 2.9–3.0 Fabrics
  7. 7. 17.11.2015 7 Pulp + acetic acid ZSK 26 Mc Acetic anhydride + catalyst Cellulose acetate < 1 min reaction time (compare with 1h in batch reactor) Esterification in Extruder
  8. 8. 17.11.2015 FTIR – Results of Acetylation 8 DS ~3.0 DS 2.4 (commercial product) DS ~2.2 DS ~0.9 normalisation to band at 1431 cm-1
  9. 9. 17.11.2015 9 Acetylated pulp, DS 0.9–1.6 Cellulose acetate, DS ~3.0NBSK pulp Pulp Acetylation in Extruder L(I) c ~ 0.2-0.5 mm L(I) c < 0.05 mm
  10. 10. 17.11.2015 10 Producing Cellulose Triacetate in Extruder Solvent casting of CTA films
  11. 11. 17.11.2015 11 Producing Acetylated Pulp in Extruder Hand sheet from acetylated pulp and its thermoplastic properties
  12. 12. 17.11.2015 12 Hand Sheets – Hot Pressing Cross-sectional SEM image of thermoplastic paper before hot pressing Cross-sectional SEM image of thermoplastic paper upon hot pressing SEM image of thermoplastic paper upon hot pressing. Fibre network structure of the non-heated area (top left) is observable
  13. 13. 17.11.2015 EXAMPLE 2 FIBRE BASED MASTERBATCHES 14
  14. 14. 17.11.2015 15 Pulp ZSK 26 Mc Various reactive modifiers/monomers Fibre-Polymer Masterbatches 1-2 min reaction time Fibre-Polymer Masterbatches in Extruder
  15. 15. 17.11.2015 Fibre-Polymer Masterbatches in Extruder 16 O O + kat. ∆ O O O H n O O O H n O O O H n + PCL
  16. 16. 17.11.2015 17 Before hot pressing Upon hot pressing Fibre-Polymer Masterbatches for Thermoplastic Paper
  17. 17. 17.11.2015 Contact Angle Measurements 18 Water drop on a NBSK + PTS-Masterbatch hand sheet, before hot pressing Water drop on a NBSK + PTS-Masterbatch hand sheet, upon hot pressing ~65° 0.5 s ~17° ~56° 0.0 s 0.5 s 0.0 s 1.0 s ~85° ~60°
  18. 18. 17.11.2015 Conclusions 19 • Reactive extrusion of cellulose fibres is a feasible way to produce cellulose derivatives, fibres and microfibrillated cellulose with added-value properties • Example 1. Cellulose acetylation • Reaction time < 1 min • Both homogeneous and heterogeneous acetylation was achieved by reactive extrusion • Various typical for cellulose acetate properties were demonstrated • Example 2. Fibre-Polymer-Masterbatches • Potential application as paper additive (thermoplastic and barrier properties) • Potential application as composite additive (as reinforcement)
  19. 19. 17.11.2015 Contact 20 Papiertechnische Stiftung, IZP Dr. Nikita Polikarpov Pirnaer Str. 37 01809 Heidenau Telefon: 03529-551-640 nikita.polikarpov@ptspaper.de http://www.ptspaper.de Papiertechnische Stiftung, IZP M.Sc. Tiemo Arndt Pirnaer Str. 37 01809 Heidenau Telefon: 03529-551-643 tiemo.arndt@ptspaper.de http://www.ptspaper.de

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