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# High Voltage Separation of Glycerol

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• GREG I need the image of the 3 grad cylinders from your paper
• Question- do the samples still have methanol?
• No glycerin in 6% for stage 1, small amount stage 2, lot in stage 3
• Add a picture of the watt meter
• Watts up? Pro Watt Meter
• Varaic- variable transformer
• NEED TALKING POINTS- is there a statistical difference between the variying ffa levels and conductivity for either biodiesel &amp; glycerin? Note the difference between biodiesel &amp; glycerin. Crude biodiesel is Dramatically different than neat biodiesel
• Goal here is characterizing the limitations &amp; conditions for the high voltage separation. What is the goal for phase 2? evaluate the change in our factors (completeness of conversion, resistance in the solution) while varying time, voltage, and oil type, and electrode distance basically we&apos;re testing the settled products (bio and glyc at 0 2 6%) to see what their baseline conductance is [11/16/09 3:32:48 PM] gbathree: then we&apos;re testing a bunch of variables, and seeing how that conductance changes over time
• Why these voltages? They were 4 settings for the variac. The variac goes from 0 - 140, but the voltage out of the wall is 0 - 120 - so if you choose seemingly normal variac settings of 5, 50, 95, 140 you end up with weird voltages after you do the calculation. the transformer is 75:1 - so you have to multiply the number by 75 to get the voltage
• 90 seconds was the cut-off, so if the bar is at 90 it did not reach the separation benchmark For all three ffa levels, when the distance between electrodes decreased, the time for separation increased. NEED TALKING POINTS: As you can see the largest distance between electrodes showed the shortest separation time for all ffa levels Higher the ffa, the longer the sep time
• NEED TALKING POINTS- but when you come separation time vs gravity, you see an apparent time variation
• Here we found that the lower limitation 1286 V which achieved 89% separation completeness
• 10 seconds is minimal level for 0% FFA 20 second is the minimal level for 6% FFA 15 second is the minimum level of 0 and 2% 20 seconds is the optimal time for all ffa levels
• What is the goal? The idea is to evaluate resistance through the medium by measuring the power through the variac, that way we can see how resistance varies as the glycerin drops out [11/16/09 3:44:44 PM] gbathree: slide 26 is sort of the key slide here
• Combine with redone exp 3 results, This is the power drop-off for 0 FFA oils. NEED TALKING POINTS
• NEED TALKING POINTS 2 % FFA oil: at varying distances, power consumption was reduced over time due to the reduction in conductance? as glycerin drops out the conductance of the material between the electrodes decreases (as we showed in the first few slides, glycerin is a better conductor)
• it looks like the big change in resistance (i.e., power) occurs once you get above 80% completeness of separation a direct comparison of completeness of conversion with power on the same graph
• Power Curve conductance shows the trend of high conductance diminishing
• ### High Voltage Separation of Glycerol

1. 1. High Voltage Separation of Biodiesel from Glycerin G. Austic, R. Burton, S. Shore, Piedmont Biofuels, Pittsboro, North Carolina, U.S.A. 2nd International Congress on Biodiesel: The Science and The Technologies 15-17 November 2009 Munich, Germany
2. 2. Background <ul><li>The goal: create a continuous separation step for biodiesel </li></ul><ul><ul><li>Graham Laming, a biodiesel enthusiast from the UK, initially discovered the phenomenon for glycerin separation from biodiesel. </li></ul></ul><ul><ul><li>Expanding on his work, we tested the following variables: </li></ul></ul><ul><ul><ul><li>electrode distances </li></ul></ul></ul><ul><ul><ul><li>separation volumes </li></ul></ul></ul><ul><ul><ul><li>container widths </li></ul></ul></ul><ul><ul><ul><li>electrode types (point, line, and screens) </li></ul></ul></ul><ul><ul><li>Eventually, we created a continuous separation device using this technology which separated 99.7% of glycerin running at 4L/min. </li></ul></ul><ul><ul><li>While the technology was interesting, we did not currently have an application, and we were concerned about the application of voltage through a methanol laden system (!). </li></ul></ul>
3. 3. Background
4. 4. Variables of Interest <ul><li>Soaps </li></ul><ul><li>FFA </li></ul><ul><li>Glycerides </li></ul><ul><li>Water </li></ul><ul><li>Viscosity </li></ul><ul><li>Voltage </li></ul><ul><li>Amperage </li></ul><ul><li>Electrode Distance </li></ul><ul><li>Container material </li></ul><ul><li>Container width </li></ul><ul><li>Container height </li></ul><ul><li>Container Length </li></ul><ul><li>Container Volume </li></ul><ul><li>Time </li></ul>
5. 5. Proposed Mechanism <ul><li>The hypothesis is that charged particles exist in the glycerin. </li></ul><ul><li>When an electric current is passed through, the charged particles line up and clump together. </li></ul><ul><li>After clumping the globule is large enough to fall out of solution. </li></ul>
6. 6. Sample Creation <ul><li>Three mini-batches were made of 0%, 2%, and 6% FFA </li></ul><ul><li>Vegetable oil was blended with Oleic Acid to create the FFA% </li></ul>FFA (%) Total Oil (mL) Virgin Oil (mL) Oleic Acid (mL) Methanol (mL) Catalyst (g) 0 200 200 0 49 1.95 2 200 196 4 49 2.72 6 200 188 12 59 4.65
7. 7. Sample Creation (cont) <ul><li>A (60/40) two-stage reaction was performed </li></ul><ul><li>The first stage was 30 minutes, the samples were heated for 2 minutes and agitated for 1 minute </li></ul><ul><li>The second stage was 1 hour, the samples were heated 4 minutes and agitated 1 minute </li></ul><ul><li>The 6% sample had an additional third stage where 0.4 g KOH in 10 mL of MeOH </li></ul><ul><li>The third stage was 30 minutes, the sample was heated for 2 minutes and agitated for 1 minute </li></ul>
8. 8. Phase 1 <ul><li>The goal was to characterize the conductivity of the glycerin and the biodiesel </li></ul><ul><li>Conductivity was calculated by measuring the power going into the transformer </li></ul><ul><li>Watts = Volts * Amperage = Amperage 2 * Ohms </li></ul><ul><li>Conductivity = 1/Ohms </li></ul><ul><li>A power meter connected the power source to the variac </li></ul>
9. 9. Watt Meter
10. 10. Phase 1 (cont) <ul><li>The variac varies the voltage entering the transformer </li></ul><ul><li>30 mL of sample was poured into a sample cup </li></ul><ul><li>The electrodes were spaced at the same height approximately 1” apart horizontally </li></ul>
11. 11. Phase 1 Results Conductivity difference between biodiesel and glycerin
12. 12. Phase 2 Set up <ul><li>The goal is to characterizing the limitations & conditions for the high voltage separation through a series of experiments </li></ul><ul><li>1. FFA and electrode distance </li></ul><ul><li>2. Low voltage limit </li></ul><ul><li>3. Minimum time </li></ul><ul><li>4. Resistance and Power </li></ul><ul><li>Biodiesel (80 mL) and Glycerin (20 mL) were mixed in a 100 mL Graduated Cylinder </li></ul><ul><li>To mix the solution, the graduated cylinder was covered with parafilm and inverted multiple times (~10) </li></ul><ul><li>Electrodes were then submerged to the proper distances and the voltage was applied </li></ul>
13. 13. Experimental Apparatus Watt Meter Variac Transformer
14. 14. Experiment 1 <ul><li>The goal was to characterize the effect % FFA and electrode distance on separation time </li></ul><ul><li>0, 2, and 6 % FFA were tested </li></ul><ul><li>Voltages of 321, 3214, 6107, and 9000 Volts were tested </li></ul><ul><li>Electrode Distances of 0.8, 5.1, 10.8, 16.5 cm were tested </li></ul><ul><li>All three FFA levels were tested at 4 voltages and 4 electrode distances </li></ul><ul><li>The voltage was stopped after 90 seconds or when 90% of the Glycerin had separated </li></ul>
15. 15. Mixed Samples Biodiesel Biodiesel Biodiesel Glycerin Glycerin Glycerin 0% 2% 6%
16. 16. Experiment 1 Results Largest distance between electrodes showed the shortest separation time for all FFA levels The higher the FFA, the longer the separation time
17. 17. Time for Gravity Settle
18. 18. Experiment 2 <ul><li>The goal was to determine the lower voltage limit </li></ul><ul><li>The farthest electrode distance was chosen along with the 2% FFA solution for better resolution </li></ul><ul><li>The voltage was applied for 40 seconds </li></ul><ul><li>Voltages tested were 321, 643, 1286, 1929, 2571, and 3214 </li></ul>
19. 19. Experiment 2 Results Lower limitation of 1286 V achieved 89% separation completeness
20. 20. Experiment 3 <ul><li>The goal was to determine the minimum time for separation </li></ul><ul><li>All three FFA levels were tested </li></ul><ul><li>The voltage was set at 9000 V and the maximum electrode distance was tested </li></ul><ul><li>The voltage was applied for set times 2, 5, 10, 15, 20, and 25 seconds </li></ul>
21. 21. Experiment 3 Results 10 seconds: 0% FFA 15 seconds: 2% FFA 20 seconds: 6% FFA
22. 22. Experiment 4 <ul><li>The goal: to evaluate resistance through the medium by measuring the power </li></ul><ul><li>The watts were recorded every 4 seconds for the 0% FFA sample and the 2 % FFA sample </li></ul><ul><li>The power was recorded until the observed wattage leveled off </li></ul>
23. 23. Experiment 4 results: 0 % FFA oil
24. 24. Experimental 4 Results: 2% FFA As glycerin drops out, conductance of the material between the electrodes decreases
25. 25. Power and Separation with Time Change in resistance (i.e., power) occurs once you get above 80% completeness of separation
26. 26. Observations/Conclusions <ul><li>Above a voltage threshold, increasing voltage provides little added benefit </li></ul><ul><li>Separation can be achieved in less than 1 minute </li></ul><ul><li>Glycerin between the two electrodes would bind to other glycerin forming globules </li></ul><ul><li>Once a globule is large enough, it falls out of suspension </li></ul><ul><li>Separation only occurs between the electrodes </li></ul><ul><li>At the higher voltages bubbling and large temperature increases were observed </li></ul>
27. 27. Next Steps <ul><li>Applying this technique in a real time system </li></ul><ul><li>Modeling the effects of electrode distance and voltage </li></ul><ul><li>Exploring the effect of heating </li></ul><ul><li>Exploring the effect methanol, soap, and water have on separation </li></ul><ul><li>Separating biodiesel, glycerin, and wash water </li></ul>
28. 28. Future Applications <ul><li>A minimum conductance difference between the liquids is required. </li></ul><ul><li>A minimum amount of charge must be able to flow through the liquids. </li></ul><ul><li>It must be a 2 phase system. </li></ul><ul><li>Applies better in viscous systems, where gravity settling is slow. However, too much viscosity could create a stable suspension. </li></ul><ul><li>Solutions with flammables pose a potential safety risk. </li></ul>
29. 29. Acknowledgements Contact: Rachel Burton Piedmont Biofuels www.biofuels.coop 919-321-8260 Piedmont Research Team: Greg Austic, Scott Shore, Xiaohu Fan