1. Recovery of Lignin Derived Phenolics
by Liquid-Liquid Extraction
Master Thesis Project
Nikolaos Montesantos
Supervisor: Marco Maschietti
K10og-5-F16

2. Agenda
• Introduction
• Hydrothermal Conversion of Biomass/Lignin
• Downstream Liquid-Liquid Extraction
• Framework
• Experimental Setup
• Experimental Procedure
• Results and Discussion
• Conclusion
2

3. Biomass
3
The Biorefinery concept [bio-economy.net]

4. Lignin
4
Lignin Facts
• Second most abundant
biopolymer
• Aromatic structures
• 100 million tones/year
Hydrothermal Conversion
• Bio-fuel
• Phenolics
Catechol
Guaiacol
Bio-crude

5. Hydrothermal Liquefaction
5
Reactor Gas
Solids
Bio Oil
Feed
Handling
Feed
Preparation
Hydrothermal
Reactor &
Separations
Liquid-Liquid
Extraction
Aqueous Phase

6. Liquid-Liquid Extraction
6
Feed
Solvent
Recovery
Extraction
Column
Organic Phase
Solvent
AqueousPhase
Recirculating Solvent
Recovered Phenolic

7. Problem Delimitation
7
Problem Definition
Develop and utilize a laboratory scale liquid-liquid extraction
method for Guaiacol by using Methyl Isobutyl Ketone (MIBK) as an
organic solvent. The method should provide accurate experimental
liquid-liquid equilibrium data for the ternary system Water-
Guaiacol-MIBK.
Literature Review
Ternary System Published Data
Water-Phenol-MIBK Yes
Water-Cresol-MIBK Yes
Water-Guaiacol-MIBK No
Water-Catechol-MIBK No
Methyl Isobutyl Ketone (MIBK) promising organic solvent for
liquid-liquid extraction

8. 8
Experimental Setup
Setup
• Temperature regulating
water bath
• Heating immersion
circulator
• Mounted separation
funnels

9. 9
Liquid-Liquid Equilibrium
1. Stock solution Water-
Guaiacol
2. Mixing with MIBK by
vigorous manual
shaking
3. Settling time 2 h
4. Sampling for
compositional analysis
5. Weighting of the two
liquid phases

10. 10
Compositional Analysis
• Gas Chromatography • Karl Fischer Titration
Organic Phase : Guaiacol
Aqueous Phase: Guaiacol & MIBK
Organic Phase: Water

11. 11
Experimental Conditions
T (°C)
Stock Solution
Composition
(wt% Guaiacol)
Different S/F ratios
Number of
Experimental
Runs
30
1 6 20
2 6 9
55
1 6 8
2 6 8
Total number of experimental runs 45

12. 12
Extraction Yield
60
65
70
75
80
85
90
95
100
0.0 0.2 0.4 0.6 0.8 1.0
ExtractionYield(%)
Solvent/Feed ratio (g/g)
1% Stock
30C 55C
60
65
70
75
80
85
90
95
100
0.0 0.2 0.4 0.6 0.8 1.0
ExtractionYield(%)
Solvent/Feed ratio (g/g)
2% Stock
30C 55C
Yield=
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑔𝑢𝑎𝑖𝑎𝑐𝑜𝑙 𝑖𝑛 𝑜𝑟𝑔𝑎𝑛𝑖𝑐 𝑝ℎ𝑎𝑠𝑒
𝑜𝑣𝑒𝑟𝑎𝑙 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑔𝑢𝑎𝑖𝑎𝑐𝑜𝑙
∙ 100

13. 13
Ternary Diagrams
30 °C 55 °C

14. Conclusion
14
• Liquid-Liquid extraction may be an effective process for the
recovery of phenolic components from aqueous streams derived by
the hydrothermal conversion of lignin
• Methyl Isobutyl Ketone is a promising organic solvents for Liquid-
Liquid extraction
• The experimental setup and procedure adopted in this project is
able to provide reliable liquid-liquid equilibrium data

15. Thank you for your attention!
Ευχαριστώ για την προσοχή σας!