Professional Documents
Culture Documents
Examination
Presented
by
Subhabrata Das
(A0109984N)
Supervisor: A/Prof. Ting Yen Peng
Department of Chemical & Biomolecular
Engineering,
National University of Singapore.
Basic Information
Title:
Demonstration of a Process for the Conversion of Kraft
520-525
Impact Factor: 2.206 (2012)
Citations: 26
2
Outline
Introduction
Methodology
Results
Critique
Suggestions for Future work
Conclusion
Introduction
Woody biomass, a renewable feedstock
for value added chemicals and biofuels
Lignin, one of the major component of
woody biomass
Kraft process generates huge amount of
lignin (72 million tons/yr) as low cost by
product (150$/ton)1
Lignin to vanillin (15000$/ton) an
attractive process2
1. Olsson, M. R.; Axelsson, E.; Berntsson, T. Nord. Pulp Pap. Res. J. 2006, 21 (4), 476484.
2. Hermans, I.; Spier, E. S.; Neuenschwander, U.; Turra, N.; Baiker. Top. Catal. 2009, 52 (9), 11621174.
Methodology
: 1g/run
: 80 vol. %
: 0.025 mol/L
: 1.13
: 170 oC
: 20 minutes
Results
A stable yield of 7 wt. % achieved after run 5
Decrease in the yield of methyl vanillate from
3.62 wt. % (run 6) to 3.27 wt. % (run 10)
Results
65 wt. % of
extracted products
retrieved after the
process reached
stability (run 6)
Critique
Key contributions:
Acid oxidation of industrial kraft lignin using H 3PMo12 O40
- To cleave alkali stable bonds
- Promising yield of 7 wt. % w as achieved higher than alkali
1. Villar, J. C.; Caperos, A.; Garcia-Ochoa, F. Wood Sci. Technol. 2001, 35 (3), 245255.
Critique
Choice of extracting solvent
Recommendation:
Ethyl acetate can be considered as an alternative
1
extracting
solvent
1. A. Vigneault, D. K. Johnson, and E. Chornet. The Canadian Journal of Chemical Engineering, 85(6):906916, 2007.
Critique
40 % of the catalyst left the system in the solid
fraction
Recommendation:
Cheap transition metal salt (CuSO4 and FeCl3) catalyst
can be considered as an alternative catalyst2
1. http://www.sigmaaldrich.com/catalog/product/sial/p7390?lang=en®ion=SG
2. Villar, J. C.; Caperos, A.; Garcia-Ochoa, F. Wood Sci. Technol. 2001, 35 (3), 245255.
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Critique
Negative values in the mass balance
11
Critique
Effect of pH and catalyst activity
Recommendation:
Change in catalyst concentration to study the effect on
yield can give a better insight on catalyst activity
12
Critique
Batch oxidation reaction
Recommendation:
Use of high pressure continuous mode micro-reactor
13
Treatment time
Operating temperature
pH
Catalyst loading
Lignin loading
Conclusion
Acid oxidation in aqueous-methanol using H3PMo12O40
resulted in promising yield of 7 wt. % of vanillin and
methyl vanillate
15
Thank You
16
Backup Slide
Redox reaction
17
Backup Slide
FT IR analysis
18
Backup Slide
Lignin production and potential lignin derived
products
19
Backup Slide
Occurrence of natural lignin
20
Backup Slide
Monolignol units
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Backup Slide
Structure of softwood lignin molecule
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Backup Slide
Most frequent linkages in lignin molecule
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Backup Slide
Biosynthesis of lignin
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Backup Slide
Kraft process
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Backup Slide
Structure of kraft lignin
26
Backup Slide
Cleavage and condensation of lignin monomers during kraft
pulping
27
Backup Slide
Potential routes of lignin utilization
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Backup Slide
Reaction network for the products during acid oxidation of
kraft lignin
29
Backup Slide
Extracted mass of lignin oxidation product from different
solvent
30
Backup Slide
Vanillin and its properties
Hocking, M. B. Vanillin: Synthetic flavoring from spent sulfite liquor. J. Chem. Educ. 1997, 74 (9), 10551059.
31
Backup Slide
Aromatic structure formed during lignin oxidation
Hocking, M. B. Vanillin: Synthetic flavoring from spent sulfite liquor. J. Chem. Educ. 1997, 74 (9), 10551059.
32
Backup Slide
Vanillin from ligno-sulphonates
Hocking, M. B. Vanillin: Synthetic flavoring from spent sulfite liquor. J. Chem. Educ. 1997, 74 (9), 10551059.
33
Backup Slide
Biomass to vanillin general pathway
Hocking, M. B. Vanillin: Synthetic flavoring from spent sulfite liquor. J. Chem. Educ. 1997, 74 (9), 10551059.
34
Backup Slide
Petrochemical method for vanillin production
Hocking, M. B. Vanillin: Synthetic flavoring from spent sulfite liquor. J. Chem. Educ. 1997, 74 (9), 10551059.
35
Backup Slide
Amount of products obtained from the oxidation of lignin in
aqueous
Voitl, T.; Rudolf von Rohr, P. Oxidation of lignin using aqueous polyoxometalates in the presence of alcohols. ChemSusChem 2008, 136
(8-9),
763769..
Backup Slide
GC-MS analysis varying catalyst concentration and solvent
concentration
Voitl, T.; Rudolf von Rohr, P. Oxidation of lignin using aqueous polyoxometalates in the presence of alcohols. ChemSusChem 2008, 137
(8-9),
763769..
Backup Slide
Effect of POM catalyst
Voitl, T.; Rudolf von Rohr, P. Oxidation of lignin using aqueous polyoxometalates in the presence of alcohols. ChemSusChem 2008, 138
(8-9),
763769..
Backup Slide
Formation of methyl vanillate from vanillin
Voitl, T.; Rudolf von Rohr, P. Oxidation of lignin using aqueous polyoxometalates in the presence of alcohols. ChemSusChem 2008, 139
(8-9),
763769..
Backup Slide
Radical coupling during lignin degradation
Voitl, T.; Rudolf von Rohr, P. Oxidation of lignin using aqueous polyoxometalates in the presence of alcohols. ChemSusChem 2008, 140
(8-9),
763769..
Backup Slide
Degradation and re-polymerization in acid condition
Voitl, T.; Rudolf von Rohr, P. Oxidation of lignin using aqueous polyoxometalates in the presence of alcohols. ChemSusChem 2008, 141
(8-9),
763769..
Backup Slide
Degradation and re-polymerization in acid condition
Voitl, T.; Rudolf von Rohr, P. Oxidation of lignin using aqueous polyoxometalates in the presence of alcohols. ChemSusChem 2008, 142
(8-9),
763769..
Backup Slide
Polyoxometalate
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Backup Slide
Effect of transition metal salts
http://e-collection.library.ethz.ch/eserv/eth:7017/eth-7017-02.pdf
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