Master in Sustainable Energies Laboratory of Biofuel Production and Characterization

Production of Biodiesel from Vegetable Oil Using Homogeneous Catalysis

INTRODUCTION
Transesterification is a process used to convert an oil or fat into methyl or ethyl esters
(biodiesel, FAME-Fatty Acid Methyl Ester or FAEE-Fatty Acid Ethyl Ester). When the oil or fat
has a high free fatty acid (FFA) content (high acidity) conversion to biodiesel is reduced.
OBJECTIVES
The objectives are:
1. To draw an experimental plan, based on DOE, that allows to find the conditions that
optimize biodiesel production;
2. To produce biodiesel, complying with the EN 14214 standard;
3. To evaluate the effect of experimental conditions on:
o Biodiesel yield;
o Biodiesel quality (density, viscosity, flash point, acid value, iodine value, CFPP,
FAME content and/or profile, water content, etc.)
4. Discuss the results obtained under different production conditions and propose
recommendation for further work.

PROCEDURE
1. Weigh 115 g of oil (or fat) into a pyrex bottle;
2. Put the Bottle in the thermostatic bath at 65 C, at a shaking speed of 80 rpm;
3. Weigh 1.1 g of potassium hydroxide in a 50 mL beaker;
4. In the hood, measure 40 cm3 of methanol (using a graduated cylinder), put it inside a
pyrex flask, add the potassium hydroxide, close the cap and then put the bottle in the
ultrasound bath until dissolution (about 5 min);
5. After dissolution, add the solution of potassium hydroxide to the hot oil bottle, in the
hood;
6. Shake it vigorously by hand, until it gets a caramel colour (5 min);
7. Put the bottle back in the shaking bath for 1 h;
8. After 1 h, remove the flask from the Thermostatic bath and pour the reaction mixture
into a separatory funnel and allow for separation of 2 phases;
9. Open the funnel and remove the bottom layer;
10. Wash the biodiesel inside the funnel using 15 cm3 of hot water to which you previously
added a few drops of phosphoric (or sulphuric) acid. Repeat the washing procedure
using only water, until the pH of water is neutral;
11. Pour the biodiesel into a beaker and add 1 g of magnesium oxide, stirring with a
magnetic bar for 10 min;
12. Filter the suspension using filtering paper and the vacuum system;
13. Store the filtered biodiesel in a previously weighed flask. Weigh again the flask with the
biodiesel and calculate the weight of biodiesel.
NSC

October 2016

Master in Sustainable Energies Laboratory of Biofuel Production and Characterization

REMARKS:
High level for temperature (A) is 70 C, whereas low level is 50 C.
High level of methanol: oil ratio is 7:1, whereas low level is 5:1.
High level of catalyst: oil ratio is 2% catalyst, whereas low level is 0.8%.
40 cm3 methanol : 115 g oil (B) corresponds approximately to 6:1 (mol methanol : mol oil).
This means that, if you are going to test for:
- 7:1 methanol: oil, you should use 47 cm3 methanol : 115 g oil.
- 5:1 methanol: oil, you should use 33 cm3 methanol : 115 g oil.
1.15 g KOH : 115 g oil (C) corresponds approximately to 1% (w/w) catalyst.
This means that, if you are going to test for:
- 2% catalyst, you should use 2.3 g KOH.
- 0.8% catalyst, you should use 0.92 g KOH.
Run

AB

AC

BC

ABC

r1

-1

-1

-1

+1

+1

+1

-1

r2

+1

-1

-1

-1

-1

+1

+1

r3

-1

+1

-1

-1

+1

-1

+1

r4

+1

+1

-1

+1

-1

-1

-1

r5

-1

-1

+1

+1

-1

-1

+1

r6

+1

-1

+1

-1

+1

-1

-1

r7

-1

+1

+1

-1

-1

+1

-1

r8

+1

+1

+1

+1

+1

+1

+1

RESULTS
Run
Volume
Weight
Density
Viscosity
Acid Value
Iodine Value
Flash Point
CFPP
HHV
NSC

October 2016