The Synthesis of Biodiesel from Waste Vegetable Oil

Abstract

In this experiment the biodiesel was synthesised from the waste vegetable oil using methanol
and sodium hydroxide (NaOH) as the catalyst. 3.5g/L of a catalyst (NaOH) was present in
lab, it was then converted to 0.35g/100 mL. To determine the amount of NaOH needed to
react with the free fatty acids in the waste vegetable oil, 1 mL of waste vegetable oil pipetted
in three conical flasks and then titrated with an excess sodium hydroxide using
phenolphthalein as an indicator, the pink colour was noticed. The average volume of sodium
hydroxide titrated against waste vegetable oil was 0.22 mL. The amount of a catalyst (NaOH)
needed to react with free fatty acids was calculated and found to be 0.08799g. The overall
amount of a catalyst used in this experiment was 0.4380g. The catalyst was dissolved in 22.2
mL of methanol, from which 100 mL of the waste vegetable oil was also added. The solution
was preheated for 30 min in the temperature if 60°C. The solution was cooled and stored in a
shelf for a week. After a week the solution showed two large phases/layers, the product (bio-
diesel) and the by-product (glyceride) at the bottom of the glass beaker. Since then the
reaction was completed the biodiesel was put in the separating funnel, a minimum of 200 mL
water was used to wash out the glycerol from biodiesel. 10 mL of dichloromethane and 3 full
spatula tips of magnesium sulphate was added in biodiesel and stirred thoroughly. The
solution was filtered and evaporated in 40°C water bath to evaporate the acid. The volume of
biodiesel was measured to be 78.5 mL, 1 mL of biodiesel was weighed to be 0.78g which is
also the value of density, from there, the mass of biodiesel was calculated to be 61.23g.
Three tests were conducted to test the quality of biodiesel. The flame test showed that the
biodiesel was flammable and it took 5 minutes and 25 seconds for it to burn in a cotton wool.
The cloud point test was performed by placing biodiesel in an ice bath where it became
highly vicious and thicker the sides of the test tube became cloudy at 13 °C. Biodiesel was
also put in a test tube with water to test for it solubility, two layers appeared in a test tube,
biodiesel at the top and water at the bottom of the test tube. This is due to the high polarity
and density of water causing the biodiesel to be insoluble in water.
Results and Discussion

Amount of a catalyst (NaOH) needed:

3.5g/L NaOH present.

Therefore, 3.5g/L × 100mL/ 1000mL × 1 L

= 0.35g/ 100mL

Table 1 Titration of 1mL sample of waste vegetable oil with 0.1 M standard solution of
NaOH

Run 1 Run 2 Run 3

Initial volume 0.53 0.74 0.96
Final volume 0.74 0.96 1.24
Volume titrated 0.21 0.18 0.28

Average volume titrated: 0.22 mL

C = n/ V

n=C×V

= 0.1 × 0.22×10-3

= 2.2 ×10-3 mol

m=n×M

= 2.2 ×10-3 × 39.997

= 8.799 ×10-4 g

8.799 ×10-3 = 1 L

Therefore, m = 0.08799 g/ 100ml

Amount of catalyst = x + 0.35g

= 0.08799 g + 0.35 g = 0.4380 g

The following is the chemical reaction for the activation of a catalyst using alcohol
(methanol):
 CH3OH+ NaOH→ CH3O- Na+ + H2O

From the calculations, 0.4380 g of the catalyst (NaOH) was accurately weighed and dissolved
in 20ml or 20% (v/ v) of waste vegetable oil. The solution was thoroughly stirred and
preheated in 60°C. The solution was then cooled at room temperature and left in a shelf for
one week. Two large phases/layers were observed after a week, product (biodiesel) at the top
and by-product glycerol at the bottom of the glass beaker.

The separating funnel was used to separate biodiesel from the glycerol. The volume of
biodiesel was measured and found to be 78.5 ml and 1 ml of it was weighed and found to be
0.78 g, which is the density per millilitre volume. Therefore,

Mass of biodiesel = d × V

= 0.78 g/ml × 78.5 ml

= 61.23 g

Fig 1. Production of Biodiesel from WVO

The stoichiometric ratio is 1: 3: 1:

The free fatty acids were formed by the process of hydrolysis reaction of triglycerides, shown
in the reaction below.
Fig 2 hydrolysis of triglyceride to form free fatty acids and glycerol

Three tests were performed to test the quality of biodiesel, mainly:

1. Flame test
5 drops of biodiesel were put in a 0.68g of cotton wool. The overall mass of biodiesel
and the biodiesel was 0.88g. the cotton wool with biodiesel was then burnt and it took
5 minutes and 52 seconds for it to burn out.

2. Solubility test
The biodiesel was placed in a test tube with water and the two layers were formed, the
biodiesel at the top and water at the bottom due to the higher density of water
compared to biodiesel. The water is more polar than biodiesel due to uneven
distribution of electrons. Therefore, the biodiesel is insoluble in water.

3. Viscosity test
the test tube containing a small amount of biodiesel was placed in an ice bath, the
biodiesel in a test tube became thick and highly viscous and the sides of the test tubes
appeared to be cloudy at the temperature of around 13°C

Discussion

the biodiesel was produced from the waste vegetable through the process called esterification.
The waste vegetable oil is typically made of triglycerides which are esters of free fatty acids
with trihydric alcohol, glycerol. In the transesterification process, the alcohol is deprotonated
with a base to make it a stronger nucleophile. Methanol was used in this experiment.

There are many tests available for the quality test of a biodiesel, others not performed in the
lab includes:

1. FFA test
The free fatty acids in a biodiesel must be less than 1 % for transesterification reaction
2. Gel test
If all the water has been removed from the product, the biodiesel should gel when
cooled
3. Methanol test
If all the WVO triglycerides were converted to into glycerol and biodiesel, then the
product should completely dissolve in methanol
4. pH test – test for the presence of NaOH, the ideal pH of a biodiesel should be around
7

a good biodiesel should also have a density ranging from 0.860 – 0.894 g/L

% volume of biodiesel = (volume of biodiesel/ volume of WVO used) × 100

 = (78.5ml /100ml) × 100

= 78.5 %

Conclusion

The experiment for the synthesis of biodiesel from waste vegetable oil was successful. The
yield of biodiesel produced from 100ml vegetable oil was 61.23g with a volume of 78.5ml.
the percentage volume of biodiesel is m78.5%. The biodiesel produced in this experiment is
of a better quality since it is flammable, highly viscous and insoluble in water. The high
percentage volume of biodiesel obtained shows that there were small errors caused during the
experiment. Since the produced biodiesel is of a good quality it can be used in standard diesel
engines and in many industries to provide energy.

References

1. Van Gerpen, J, 2005, Biodiesel processing and production. Fuel processing

technology, 86(10), pp.1097-1107.
2. “Biodiesel to drive up of cooking”, Biopower London, 2006, Retrieved 2008-04-03
3. Van Gerpen, John, (2004 – 2007), “Business Management for biodiesel producers”,
august 2002 – January 2004”, (PDF). National Renewable Energy Laboratory,
Retrieved, 07-01-2208.
 PRODUCTION OF BIODIESEL
FROM WASTE VEGETABLE
OIL
FINAL REPOT

Name: Mxolisi Simosethu

Surname: Mtshali

Student no.: 216006704