CHAPTER III CHAPTER III
IV 3.2 IV 3.2 Problem Statement
4.3 Experimental Procedure
F
4 f Table 4. 1: Reaction Parameters
Reaction Parameters Esterification Transesterification
Oil:Methanol 1.02:6.6 1.02:6.6
Catalyst Conc. 3 wt% (H2SO4) of castor oil 0.5 wt% (NaOH) of castor oil
Temperature 45-70°C 45-70°C
Time 3 hrs 3 hrs
After the reaction, the reaction mixture should be allowed to cool and settle in measuring cylinder. The settling period allows for the reaction mixture to separate into the two products namely glycerol and the biodiesel. The separation occurs over a period of about 7 or more hours. A photographic view of measuring cylinder is shown in Figure 4.6.
Figure 4.6: Photographic view of measuring cylinder
Measuring Cylinder was used to measure the amount of biodiesel and glycerol after layer separation.
The methodology developed / processes adopted for production of biodiesel was given below.
Whole process was described for one liter of castor oil. During processing of multiple quantity of castor oil, chemical constituents were changed in the same proportion however timing for heating, settling and washing remain same.
First step
• One liter of castor oil was taken into the Reactor.
• 250 ml of methanol & 16 ml of concentrated sulphuric acid was added to oil.
• The temperature of this mixture was maintained 45°C to 70°C and data was collected at every 5°C temperature interval.
• This temperature of the mixture was maintained for about 3 hours and stirred continuously.
• The mixture was allowed to settle for 8 hours after completion of this reaction and cooling the reaction mixture.
Second step
• 5g NaOH was added to oil mixture.
• This temperature of the mixture was maintained 45°C to 70°C and data was collected at every 5°C temperature interval.
'The mixture stirred continuously for about 3 hours.
Chemical reaction of Triglyceride with Methanol is shown below.
0 11 CH2O-C-R1
O CH2-01-1 CH3COOR1
I I Catalyst
CH-O-C-R2 + 3 CH3 OH CH-OH + CH3COOR2
I 0
I CH2 —OH CH3COOR3
CH2-O-C-R3
Triglyceride Methanol Glycerol Methyl Ester (Biodiesel)
37
• The mixture was collected from reactor after reaction completion.
-The mixture was allowed to settle for 8 hours in separating bottle. This settled reactant mixture would consist of two layers.
Upper layer as biodiesel and traces of glycerin etc.
Bottom layer as glycerin and gums etc.
A photographic view of biodiesel and glycerol separation is shown in Figure 4.7.
Figure 4.7: Photographic view of biodiesel and glycerol separation
• The Biodiesel was collected from the separating bottle by using pipette and filler.
• The biodiesel separated in this stage still impure and needs to be bubble washing. This pre- washed biodiesel was taken in a washing vessel. Water was added in washing vessel as 2:1 ratio of biodiesel.
• This process involves cleaning the fuel with water by using agitation which was provided by compressed air through the water and biodiesel mixture.
•After bubble wash this mixture should be allowed more than 8 hours for settle down. After two layer separation biodiesel was collected in beaker.
•For further purification 600 ml of hot water at approximately 40° C was added per liter of crude biodiesel in separating bottle and shaken well and allowed to settle to separate two layers for nearly 7-8 hours.
• Above process was repeated two times so that the traces of glycerin and soap get removed and the biodiesel produced from castor oil was ready for use. A Photographic view of Methyl Ester (Biodiesel) was produced from castor oil is shown in Figure 4.8.
Figure 4.8: Photographic view of Methyl Ester (Biodiesel) 4.4 Experimental Data
During the experiments. Castor oil was charged in the reactor chamber in different ratio of castor oil and methanol. Details of Sample was used in various run is shown in Table 4.2.
Table 4.2: Details of Sample was used in various run.
Sample NO. Castor Oil Methanol Molar ratio=
Castor Oil : Methanol
Total Volume Liter Mole Liter Mole (L)
1 3.0 1.02 1.0 8.23 1.02: 8.23 4.00
2 2.8 0.96 0.85 7.00 0.96: 7.00 3.65
3 2.9 0.98 0.73 6.00 0.98: 6.00 3.63
4 3.0 1.02 0.75 6.17 1.02: 6.17 3.75
5 3.0 1.02 0.80 6.60 1.02: 6.60 3.80
V
The experiments were performed by varying the temperature within the range of 45-70°C at every 5°C interval for each feed. The data collected during esterification and 1 transesterification of castor oil to biodiesel shown in Table 4.3 through 4.12.
Table 4.3: Experimental data for esterification of 4.0 liter feed Materials for Various Temperatures using H2SO4 as catalyst.
Sample-I: (3 wt% H2SO4 as catalyst) Feed Materials: 4.00 Liter, ,Molar ratio= 1.02: 8.23
No. of Observation
Temperature (°C)
Product yield, L Operating Time biodiesel Unreacted
feed
glycerol
1 45 1.20 2.69 0.110 50
2 50 1.40 2.47 0.135 75
3 55 1.65. 2.21 0.144 100
4 60 2.00 1.85 0.150 125
5 65 2.32 1.53 0.155 150
6 70 2.31 1.53 0.160 175
Table 4.4: Experimental data for esterification of 3.65 liter feed Materials for Various Temperatures using H2SO4 as catalyst.
Sam ple-2: (3 wt% H2SO4 as catalyst) Feed Materials: 3.65 Liter, Molar ratio= 0.96: 7.00
No. of Observation
Temperatur e (°C)
Product yield, L Operating Time biodiesel Unreacted
feed
glycerol
1 45 1.02 2.54 0.095 50
2 50 1.22 2.33 0.105 75
3 55 1.45 2.09 0.114 100
4 60 1.74 1.785 0.125 125
5 65 2.15 1.36 0.137 150
6 70 2.14 1.36 0.145 175
'1'
Table 4.5: Experimental data for esterification of 3.629 liter feed Materials for Various Temperatures using H2SO4 as catalyst.
Sample-3: (3 wt% H2SO4 as catalyst) Feed Materials: 3.63 Liter, Molar ratio= 0.98: 6.00
No. of Observation
Temperature (°C)
Product yield, L Operating Time (mm) biodiesel Unreacted
feed
glycerol
1 45 1.12 2.42 0.090 50
2 50 1.22 2.31 0.102 80
3 55 1.44 2.08 0.110 110
4 60 1.72 1.79 0.122 140
5 65 2.14 1.35 0.140 170
6 70 2.13 1.35 0.148 200
Table 4.6: Experimental data for esterification of 3.85 liter feed Materials for Various Temperatures using H2SO4 as catalyst.
Sample-4: (3 wt% 112SO4 as catalyst) Feed Materials: 3.75 Liter, Molar ratio= 1.02: 6.17
No. of Observation
Temperature (°C)
Product yield, L Operating Time (miii) biodiesel Unreacted
feed
glycerol
45 1.16 2.45 0.092 50
2 50 1.24 2.40 0.106 80
3 55 1.48 2.16 0.112 110
4 60 1.90 1.73 0.125 140
5 65 2.25 1.37 0.134 170
6 70 2.24 136 0.144 200
41
Table 4.7: Experimental data for esterification of 4.7 liter feed Materials for Various Temperatures using H2SO4 as catalyst.
Sample-5: (3 wt% H2SO4 as catalyst) Feed Materials: 3.80 Liter, Molar ratio= 1.02: 6.60
No. of Observation
Temperature (°C)
Product yield, L Operating Time (mm) biodiesel Unreacted
feed
glycerol
1 45 1.17 2.53 0.096 50
2 50 1.27 2.42 0.110 80
3 55 1.50 2.19 0.114 110
4 60 2.00 1.68 0.124 140
5 65 2.28 1.39 0.135 170
6 70 2.27 1.38 0.146 200
Table 4.8: Experimental data for transesterification of 4.0 liter feed Materials for Various Temperatures using NaOH as catalyst.
Sample-6: (0.5 wt% NaOH as catalyst) Feed Materials: 4.00 Liter, Molar ratio= 1 .02: 8.23
No. of Observation
Temperatur e (°C)
Product yield, L Operating Time (mm) biodiesel Unreacted
feed
glycerol
1 45 2.35 1.49 0.165 50
2 50 2.60 1.23 0.175 75
3 55 2.80 0.98 0.215 100
4 60 3.12 0.63 0.245 125
5 65 3.40 0.34 0.264 150
6 70 3.39 0.34 0.270 175
4.9: Experimental data for transesterification of 3.65 Liter feed Materials for Various Deratures using NaOH as catalyst.
Sample-7: (0.5 wt% NaOH as catalyst) Feed Materials: 3.65 Liter, Molar ratio= 0.96: 7.00
No. of Observation
Temperatur e (°C)
Product yield, L Operating Time (miii) biodiesel Unreacted
feed
glycerol
45 2.25 1.25 0.150 50
2 50 2.41 1.08 0.156 75
3 55 2.63 0.86 0.162 100
4 60 3.00 0.43 0.220 125
5 65 3.20 0.20 0.255 150
6 70 3.19 0.19 0.262 175
Table 4. 10: Experimental data for transesterification of 3.63 liter feed Materials for Various Temperatures using NaOH as catalyst.
Sample-8: (0.5 wt% NaOH as catalyst) Feed Materials: 3.63 Liter, Molar ratio= 0.98: 6.00
No. of Observation
Temperature (°C)
Product yield, L Operating Time biodiesel Unreacted
feed
glycerol
1 45 2.25 1.23 0.152 50
2 50 2.50 0.97 0.162 80
3 55 2.72 0.73 0.185 110
4 60 2.94 0.48 0.214 140
5 65 3.19 0.19 0.250 170
6 70 3.18 0.19 0.260 200
43
Table 4.11: Experimental data for transesterification of 3.85 liter feed Materials for Various Temperatures using NaOH as catalyst.
Sample-9: (0.5 wt% NaOH as catalyst) Feed Materials: 3.75 Liter, Molar ratio= 1.02: 6.17
No. of Observation
Temperature (°C)
Product yield, L Operating Time (miii) biodiesel Unreacted
feed
glycerol
1 45 2.35 1.25 0.150 50
2 50 2.55 1.04 0.160 80
3 55 2.96 0.63 0.165 110
4 60 3.18 0.37 0.205 140
5 65 3.37 0.15 0.228 170
6 70 3.36 0.14 1 0.246 200
Table 4. 12: Experimental data for transesterification of 4.7 liter feed Materials for Various Temperatures using NaOH as catalyst.
Sample-lO: (0.5 wt% NaOH as catalyst) Feed Materials: 3.80 Liter, Molar ratio= 1.02: 6.60
No. of Observation
Temperature (°C)
Product yield, L Operating Time biodiesel Unreacted
feed
glycerol
1 45 2.40 1.25 0.152 50
2 50 2.62 1.02 0.163 80
3 55 2.96 0.66 0.184 110
4 60 3.26 0.33 0.214 140
5 65 3.42 0.14 0.238 170
6 1 70 3.41 0.13 0.258 200
CHAPTER V
RESULTS AND DISCUSSION