Optimising the Conversion of

Waste Cooking Oil into Biodiesel

Supervisor: Dr. Watson
Biodiesel: a fuel comprising mono-
alkyl esters of long chain fatty acid.
Derived from vegetable oils or animal
fats. Designated B100

Important Properties:
Cloud point
Viscosity
Alkyl esters concentration
Monitored and evaluated in this project

29th August 2008

 Feedstock for Biodiesel

Virgin Vegetable Oil: rapeseed oil, soybean oil,

cotton oil, sunflower seed
Cost decrease

Free fatty acid decrease

Waste Cooking Oil: yellow grease, brown
grease

Animal Fat: tallow, fish fat

(triglyceride: TG and free fatty acid FFA)

New feedstock under study:

Different kinds of Marine Algae

29th August 2008

 Four Methods to Derivatize
Vegetable Oils into Biodiesel

Dilution: Blending with pure ethanol to reduce viscosity

Microemulsion: Blending various vegetable oils with conventional
fuel to decrease viscosity

Pyrolysis: Thermal decomposition of vegetable oils to diminish the

viscosity

Alcoholysis: Reaction of vegetable oils or animal fats with a short

chain alcohol to derivatize the triglycerides and fatty acid into esters -
to lower viscosity
 Biodiesel Production Processes

Acidic Esterification Equation

Catalyst: H2SO4
Alcohol to FFA molar ratio >15:1

Basic Transesterification
Equation
Catalyst: NaOH
Alcohol to TG ratio >6:1

29th August 2008

 Materials and Equipment

Materials: Waste cooking oil

Pure methanol
98% H2SO4
Sodium hydroxide pellets
Ethyl acetate as GC sample solvent

Equipment: Gas chromatography machine

IR spectrometry
Balance
U tube
Thermometer
Separation funnel

29th August 2008

 Acid Value Determination

 Determined according to BP monograph

 Evaluate the weight of FFA and TG in the
waste cooking oil
 Estimate the proper amount of catalysts and
methanol needed in biodiesel production
The quality of the waste cooking oil can be very different !!!

Benefits: Help to increase the conversion rate

of methyl esters and decrease the chance of
soap formation and cost

29th August 2008

 Viscosity and Cloud Point Comparisons between
Lab Biodiesel Groups and Control Groups
Groups Cloud Point Sample Nos Groups Viscosity Sample Nos
Lab 11.57°C 27 Lab 11’34” 27
Control 11°C 5 Control 12’19” 5

Boxplot of cloud point C, cloud point B Boxplot of relative viscosity C, relative viscosity B

13.0 14

12.5
13

12.0
12
Data

Data
11.5
11
11.0

10
10.5

9
10.0

cloud point C cloud point B relative viscosity C relative viscosity B

2 sample t-test for both = no difference !!

29th August 2008
 IR and Standard Methyl Esters GC Tests
Identify: standard methyl palmitate GC calibration y = 673191x + 4515.6
R2 = 0.9981

IR and esters retention time on GC

800000
700000
600000

peak area
500000

Generate Calibration Equation: 400000

300000

C (16:0), C (18:0) & C (18:1) methyl

200000
100000

esters
0
0 0.2 0.4 0.6 0.8 1 1.2

concentration

standard methy oleate GC caliration standard methyl stearate GC calibration y = 594587x + 3553.7
y = 625704x + 2614
R2 = 0.9979 R2 = 0.995
700000 700000
600000 600000
500000 500000
peak area

peak area
400000 400000
300000 300000
200000 200000
100000 100000
0 0
0 0.2 0.4 0.6 0.8 1 1.2 0 0.2 0.4 0.6 0.8 1 1.2
concentration concentration

29th August, 2008

 2 Sample t-test to Evaluate the GC
Experiments of Grouped Biodiesel Samples
Methyl esters GC results among different stages Methyl esters GC results between 2 groups
Stage Total esters RSD Groups Esters conc. Sample Nos
(mg/ml) Mg/ml
Acidic 0.01070. 6.7% Lab 0.7243 27
Basic 0.2441 2.8%
Controlled 0.6923 5
Optimized 0.7742 3.2%

Boxplot of controlled group, lab batches

2 sample t-test: better 0.90

Conversion rate of esters

0.85

using the optimized

0.80

method
Data

0.75

0.70

0.65

0.60
controlled group lab batches

29th August, 2008

 Conclusion: Optimized Method is Better!
Summary of Optimised Method:
Step 1: Determine acid value
Step 2: Heat oil and remove water
Step 3: Acidic esterification: heat to 50C, add 0.5 - 1.0% H2SO4,
mix with 1:15 - 1:20 molar ratio of FFA to methanol

Step 4: Prepare sodium methoxide solution 30mg/ml

Step 5: Basic transesterification: heat to 60 C, add 16 - 18%
sodium methoxide by weight of TG in waste cooking oil to feedstock

Step 6: Separate the top and bottom layers

Step 7: Wash with warm water

Xiaoming Chen dustinchen@gmail.com MSc (Pharmaceutical Analysis) University of Strathclyde

29th August 2008