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Figure: XRD pattern of natural eggshell and materials obtained by calcining natural eggshell
in range of 200 C C.
Eggshell sample calcinated at 900 C provides the most active catalyst with yield of 96%.
When calcination take place at higher temperature, it led to desorption of carbon dioxide
from egg shell catalysts which decrease biodiesel yield to 90%. A yield of 9799% was
obtained when eggshell sample calcinated above 800 C and yield dropped to 90% when the
calcination temperature was 700 C.
II.
Reaction temperature
From the figure above, we can see increase in reaction temperature have two opposite
effects. At first, an increase in the temperature will increase the rate of reaction due to a
higher energy input and a reduced mass transfer resistance. When the temperature is
greater than 65 C results in negative effects as it exceeds the boiling point of methanol. This
results in decrease of methanol solution as most of the methanol remain in vapour phase.
Hence, the yield of biodiesel yield was increased with an increase in temperature of up to
65 C, optimum. A yield of 94.49% for chicken egg shell can be obtained at 65 C operating
temperature.
IV.
Catalyst concentration
From the figure, increase in alcohol/oil molar ratio and catalyst amount at first leads to
increase in biodiesel yield at a maximum of 9:1 methanol to oil molar ratio with 3wt%
eggshell catalyst before the trend was reversed. Increasing the catalyst amount more than
3wt% will result in poor mixing of the reaction mixture comprising solid (catalyst), non-polar
(vegetable oil and biodiesel yield) and polar (methanol) phases. Hence, aggregation of
catalysts and poor mass transfer between phases reduced biodiesel yield. Similarly, excess
methanol will shift the equilibrium to the right and improve biodiesel yield, but beyond a
certain value the excess methanol causes dilution. Catalyst concentration with respect to the
volume of reaction mixture decreased with an increase in methanol concentration which
then caused a drop in biodiesel yield.
V.
Reaction time
Based on the figure above, the maximum yield of FAME we are able to obtained is 94.49% in
4 hours at 60C for chicken egg shell. We can see that the yield increase in time from 1 to 4
hours with catalyst amount of 20wt% and a methanol/oil molar ratio of 9:1. As the residence
time more than 4 hours, the rate decreases. This can be explained by that transesterification
reaction between oil and alcohol is reversible when reaction time is long enough.
VI.
Catalyst recyclability
Based on the diagram below, eggshell-derived catalyst can be repeatedly use for 13 times
without any apparent loss of activity for transesterification. The catalyst gradually loses its
activity after being used for more than 13 times. The catalyst was completely deactivated
after being used more than 18 times. The deactivation of mixture catalyst may be ascribed
to its structure change. The XRD patterns of the eggshell- derived catalyst used more than
18 times were characteristic of Ca(OH)2. The structure change of catalyst could result from
the reaction between H2O and CaO, because the reactants (vegetable oils and methanol)
contain a little amount of water.
VII.
Catalyst size