Insights into Eucalyptus Pulp Bleaching Technology

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1 Insights into Eucalyptus Pulp Bleaching Technology Tapani Vuorinen 6th International Colloquium on Eucalyptus Pulp Colonia del Sacramento, Uruguay November 24-27, 2013

2 Outline From present to future Maintaining fiber properties Does chemistry help? Conclusions

3 Outline From present to future Maintaining fiber properties Does chemistry help? Conclusions

4 Main targets of pulp bleaching To reach high brightness Low lignin chromophore content To reach high brightness stability Low residual lignin content Low hexenuronic acid (HexA) content Low carbonyl content To remove most of chromophores, lignin and HexA without oxidizing polysaccharides

5 Approximate composition of oxygen delignified eucalyptus kraft pulp Cellulose + hemicelluloses (excluding HexA) 98 m-% 6,250 mmol/kg (anhydrosugar units) 17,500 mmol/kg (hydroxyl groups) 12,500 mmol/kg (accessible hydroxyl groups) Hexenuronic acid (chemically bonded to xylan) 1 m-% 65 mmol/kg Lignin (chemically bonded to polysaccharides) 1 m-% 50 mmol/kg (phenylpropane (C 6 C 3 ) units)

6 Characteristics of high quality bleached eucalyptus kraft pulp Cellulose + hemicelluloses (excluding HexA) > 99.5 m-% < 10 mmol/kg carbonyl groups high accessibility Hexenuronic acid < 0.1 m-% Lignin < 0.1 m-%

7 ECF bleaching sequences of oxygen delignified eucalyptus kraft pulp A/D-E OP -D-P or D/A-E OP -D-P kg active Cl/ton mmol/kg (ClO 2 ) mmol/kg (act. Cl 2 ) 7-10 kg hydrogen peroxide/ton mmol/kg (H 2 O 2 ) A-E OP -D-P kg active Cl/ton 80 mmol/kg (ClO 2 ) 200 mmol/kg (act. Cl 2 )

8 Inefficiency in current ECF bleaching technology Long retention times huge bleaching towers Excessive oxidation power needed in removal of residual lignin and HexA 4-6 equivalents of oxidant per C 6 C 3 + HexA 7-9 equivalents of oxidant per C 6 C 3 + HexA (HexA hydrolyzed by acid calculated out) Target should be in doubling the efficiency!

9 Outline From present to future Maintaining fiber properties Does chemistry help? Conclusions

10 Irreversible deuteration of cellulose in kraft pulping of birch 1) Pulping in D 2 O 2) Washing with H 2 O 3) Detection of OD band Raili Pönni et al. Carbohydrate Polymers 101 (2014)

11 FTIR spectra of HW pulps cooked in D 2 O and H 2 O Raili Pönni et al. Carbohydrate Polymers 101 (2014)

12 Irreversible deuteration of eucalyptus pulps treated for 4 hours at 90 o C 1) Treatment in D 2 O 2) Washing with H 2 O 3) Detection of OD band Raili Pönni et al. Carbohydrate Polymers 93 (2013)

13 FTIR spectra of eucalyptus pulp treated for 4 hours in D 2 O at 90 o C OD Raili Pönni et al. Carbohydrate Polymers 93 (2013)

14 Factors affecting on hornification of pulp = aggregation of cellulose microfibrils Cooking: removal of hemicelluloses and high temperature + long time Bleaching: high temperature and long time Drying: removal of water during long time at high temperature Using lower temperature and faster reactions could reduce hornification in bleaching

15 Outline From present to future Maintaining fiber properties Does chemistry help? Conclusions

16 UV Raman spectra of bleached kraft pulps Kristiina Kellokoski M.Sc. Thesis 2013

17 General reaction scheme of chlorine dioxide bleaching

18 Oxidants in chlorine dioxide bleaching Chlorine dioxide (ClO 2 ) Oxidizes phenols and hydroxyquinones (2 equivalents ClO 2 per phenol or hydroxyquinone) Produces ½ equivalents HOCl and ½ equivalents ClO 2 - Chlorite (ClO 2- ) Oxidizes aldehydes (formed in situ) forming equivalent amount of HOCl Decomposes to chlorate (ClO 3- ) and HOCl (catalysis by HOCl) May react with HOCl to regenerate ClO 2 Hypochlorous acid (HOCl) Oxidizes HexA Chlorinates and oxidizes lignin Oxidizes cellulose and hemicelluloses

19 Stoichiometry of overall reactions 2ArOH + HexA + 4ClO 2 2Ox Lig + Ox HexA + ClO Cl - In this simplified (but relevant) scheme HexA and lignin are oxidized in a 1:2 ratio! Formation of HOCl in situ equivalents per added ClO mmol/kg pulp, when total active Cl charge is kg/ton Formation of chlorate (ClO 3- ) equivalents per added ClO mmol/kg pulp, when total active Cl charge is kg/ton

20 Reactivity of HOCl Electrophilic reactions Primary oxidation of HexA - OK Chlorination of lignin reduces reactivity of residual lignin (by factor of 10 per each substitution) Oxidation of lignin - OK Oxidation of cellulose and hemicelluloses may decrease brightness stability Nucleophilic reactions Secondary oxidation of HexA consumes oxidant without promoting removal of HexA Oxidation of chromophores - OK

21 Reactivity of HOCl

22 Effect of carbonyl content on brightness reversion of ECF bleached eucalyptus pulp PC, 48h ageing reference pulp (xylan 12%) hemicellulose-reduced pulp (xylan 7%) Original pulp Brightness reversion is only caused by carbonyl groups! Carbonyl content, mol/g Zhen Zhou et al. Holzforschung 65 (2011)

23 UVRR spectra of eucalyptus kraft pulps in A-E OP -D-P bleaching sequence HexA Lignin Cellulose Leonardo Clavijo M.Sc. Thesis 2010

24 Derivatives of HOCl (Cl 2 ) General reaction (nucleophilic substitution on chlorine): Nu - + Cl + -Cl - Nu-Cl + Cl - Nucleophile Product Name H 2 O/HO - HOCl Hypochlorous acid ClO - Cl 2 O Chlorine monoxide ClO - 2 Cl 2 O 2 Dichlorine dioxide RCO 2 H RCO 2 Cl Acyl hypochlorite ROH ROCl Alkyl hypochlorite ArOH ArOCl Aryl hypochlorite R 3 N R 3 N + Cl Chloroammonium cation

25 Outline From present to future Maintaining fiber properties Does chemistry help? Conclusions

26 Conclusions Eucalyptus pulp bleaching could and should be intensified from today s BAT In the future bleaching can be dramatically faster than today and consume much less chemicals In addition to lower investment and production costs the new technology may better maintain beneficial fiber properties

27 Acknowledgements Long-term financers and idustrial collaborators: TEKES (Finnish Funding Agency for Technology and Innovation) Finnish Bioeconomy Cluster Ltd (Strategic Centre for Science, Technology and Innovation) Andritz, Metsä Fibre, Kemira, Stora Enso, UPM Research collaborators during the past years: Aalto University BOKU INPG Pagora Universidad de la República VTT

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