Supercritical Fluid Extraction of Caffeine from Pyrolyzed Coffee Ground Bio-oil

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Supercritical Fluid Extraction of Caffeine from Pyrolyzed Coffee Ground Bio-oil Osariemen Ogbeide (PhD candidate) (Paul Charpentier and Mita Ray)

1 Supercritical Fluid Extraction of Caffeine from Pyrolyzed Coffee Ground Bio-oil Osariemen Ogbeide (PhD candidate) (Paul Charpentier and Mita Ray) Western University, London, ON, Canada An HQP Perspective on Emerging and Advanced Biofuel Technologies Advanced Biofuels Symposium, July 2015, Montreal 1

2 Project 6 Synergies Woody Biomass Carbohydrates Acid Catalysis 5-HMF Wastewater Flue Gas Waste Fats and Oils Yeast and Algae Fermentation Lipid-to-Hydrocarbon SEES Biosolids Ionic Solventbased Extraction CO 2 -based Extraction Lipids Hydrogenation & Catalysis Hydrothermal Liquefaction Biofuels Acid Precipitation & Electrodialysis Kraft Black Liquor Lignin Wet Biomass Acidification Co-products 2

3 Outline Background Objectives Methods Results Conclusion Future works 3

4 Background Phase diagrams of carbon dioxide Isotherms: (A) 177 C (B) 127 C (C) 77 C (D) 27 C and (E) -23 C, respectively 4

5 Objectives Bio-oil Characterization (GC-MS, HPLC) Modeling SFE of caffeine (CO 2, ethanol, methanol) 5

6 Methods PFD of the SFE system. Basic components: high pressure valves, (V1-V9); high Pressure check valves, (CV1-CV3); temperature controllers, (TC1-TC3); and pressure controllers, (PC1-PC2). 6

7 Methods Determination of caffeine yield Caffeine yield wt. % = Mass of extracted caffeine g Mass of caffeine rich extract g Second order polynomial model Y = β 0 + β i X i + β ii X i 2 + β ij X i X j i=1 i=1 i=1 j>1 (2) Here, Y, t, T, P correspond to the predicted caffeine yield (wt. %), time (min), temperature (K), pressure (MPa), respectively. Prediction of binary diffusivity (modified Wilke-Chang equation) D 12 = at MW 2 μbv 1 (3) Here, a and b are constants; V 1 is the molar volume of caffeine at boiling point ; μ corresponds to the viscosity of CO 2 at specified T, P; MW 2 is the molecular weight of carbon dioxide. 7

8 Results (Characterization of coffee ground bio-oil) Caffeine content: GC-MS Area% = 9.7 % and yield from HPLC = 3 wt.% (a) (b) (a) Gas chromatography with mass spectrometry (GC-MS) chromatogram (b) High performance liquid chromatography spectra. 8

9 Prediction of caffeine diffusivity in SC-CO 2 (modified Wilke-Chang equation) (a) Effect of CO 2 pressure on diffusivity of caffeine (b) Effect of CO 2 density on diffusivity of caffeine The lines above represents the calculated data, shapes are literature data adapted from Lai et al. (1995) 9

Measurements of extraction curves around the optimum using pure SC-CO 2 Response Surface Optimization SC-CO 2 extraction Experiment (a) Effect of SFE-CO 2

10 Measurements of extraction curves around the optimum using pure SC-CO 2 Response Surface Optimization SC-CO 2 extraction Experiment (a) Effect of SFE-CO 2 process variables: (a) Pressure and temperature obtained from RSO. (b) pressure; 20 min extraction time on caffeine extraction from coffee ground bio-oil (b) 10

11 Measurements of extraction curves around the optimum using modified SC-CO 2 Effect of co-solvents on caffeine extraction as a function of pressure 11

12 Conclusions Bio-oil was characterized by GC-MS and HPLC analysis leading to a high caffeine content of around 3 wt. %. Diffusivity of caffeine in the SC-CO 2 phase was calculated using a modified Wilke- Chang equation and the results were close to experimental data from open literature. Response surface methodology was capable of finding the optimum process variables (333 K, 35.2 MPa and 20 min), for caffeine isolation from the caffeine rich bio-oil. The addition of co-solvent (10 % ethanol) to supercritical CO 2 could recover a maximum of 22 wt. % of caffeine from bio-oil at optimum condition. 12

13 Future works Production and characteriza tion of biosurfactant Bio-diesel production Algae Characterize algae (GC and HPLC) SFE of lipids (CO 2, Cosolvents) 13

14 Acknowledgements Prof. Paul Charpentier Prof. Mita Ray Prof. Franco Berruti Prof. Cedric Briens Mohammad Hossain Colleagues at Western University 14

15 Thank you for listening! 15

THE FOLLOWING TEXT ON BIO-OIL EXTRACTION IS AN EXCERPT FROM THE FINAL TECHNICAL REPORT SUBMITTED BY HNEI TO OFFICE OF NAVAL RESEARCH UNDER GRANT

THE FOLLOWING TEXT ON BIO-OIL EXTRACTION IS AN EXCERPT FROM THE FINAL TECHNICAL REPORT SUBMITTED BY HNEI TO OFFICE OF NAVAL RESEARCH UNDER GRANT AWARD NUMBER N00014-09-1-0709, DECEMBER 2011 2.4 Novel Solvent-Based