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Biodiesel Synthesis Experimental Procedure


Equipment:

  • 250ml beaker (x2)
    Biodiesel mixture.JPG
    Biodiesel Mixture
    Biodiesel Sodium Methoxide.jpg
    Sodium Methoxide
  • 100ml graduated cylinder
  • 50ml graduated cylinder
  • 250ml separatory funnel
  • Ring stand with ring (x2)
  • Magnetic stir plate with magnet stir rod
  • Lamp wick
  • 10ml graduated cylinder
  • Wire mesh
  • 250ml volumetric flask
  • Soda can
  • Aluminum foil
  • lighter
  • Thermometer

Pre-experiment calculations:

  • 3.5g NaOH per 1L oil
  • 9.0g KOH per 1L oil
  • 20% Methanol per volume of oil
  • 30% Ethanol per volume of oil


Reagents:

  • 100ml Canola oil
  • 100ml Vegetable oil
  • 0.35g NaOH
  • 0.90g KOH
  • 20ml Methanol
  • 30ml Ethanol

The Reaction:

Biodiesel reaction.jpg
Biodiesel Synthesis Reaction (Thompson, 2006)



Procedure:

Biodiesel Synthesis

  1. Add measured catalyst (NaOH or KOH) to measured alcohol (Methanol or Ethanol) in 250ml Beaker with magnetic stir bar and stir until all of the catalyst has dissolved.
  2. (if desired) Warm oil to approximately 40 degrees C. This is not a requirement for the reaction to occur, but will increase the reaction rate.
  3. Add the oil to the catalyst/alcohol mixture. Stir for 30 minutes.
  4. Transfer the mixture from the beaker to the separatory funnel. Allow the biodiesel and glycerol to separate for 1-24 hours. The glycerol will form the bottom layer, with the biodiesel forming the top layer.
  5. Drain glycerol and biodiesel into separate containers (be careful to not mix glycerol and biodiesel).

Biodiesel Calorimetry

  1. Setup ring on ring stand with wire mesh to hold the soda can and thermometer.
  2. Fill 10ml graduated cylinder with 5ml biodiesel, insert wick, rotate and tilt to completely saturate wick with biodiesel.
  3. Fill soda can with exactly 250ml room temperature water, place on ring stand with thermometer, record initial temperature.
  4. Fill 10ml graduated cylinder with approximately 6-9ml biodiesel, record initial volume.
  5. Place 10ml graduated cylinder under the soda can so that the tip of the flame will be at the bottom of the can. Use the foil to create a heat shield around the graduated cylinder to help contain the heat.
  6. Light the wick and monitor the temperature, occasionally stirring the water to ensure even heat distribution, once the water has increased in temperature by 10 degrees C extinguish the flame, record the maximum temperature of the water (it may continue to rise immediate after removing the flame).
  7. Record the final volume of the biodiesel.
  8. Repeat two times, using fresh room temperature water.

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Biodiesel in separatory funnels.JPG
Biodiesel Separatory Funnel (initial)
Biodiesel in separatory funnel (24hr).jpg
Biodiesel Separatory Funnel (24 hours)




















Biodiesel calorimetry.jpg
Biodiesel Calorimetry Test Setup



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References:

University of California, Berkeley. (2014). Biodiesel Heat of Combustion and Energy Efficiency. The Berkeley Center for Green Chemistry. Retrieved from http://www.bcgc.berkeley.edu/sites/default/files/GreenChemistry_Biofuels_Unit.pdf

Thompson, J., (2006), Biodiesel Synthesis. Lane Community College Science Division, Retrieved from http://greenchem.uoregon.edu/PDFs/GEMsID87.pdf