1. Jidon Janaun1, Naoko Ellis2,
Controlled functionalization of amorphous carbon using multiple vapour phase sulfonation for production of biodiesel
Jidon Janaun1, Naoko Ellis2,
Kevin J. Smith2
1Universiti Malaysia Sabah
2University of British Columbia, Canada

2. Outline Introduction to biodiesel & sugar catalyst
Preparation of mesoporous carbon-based catalyst
Multiple vapour phase sulfonation
Catalytic activity on esterification of oleic acid
Conclusions
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

3. Biodiesel synthesis
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

4. Selection of Feedstock
- Readily available in large quantity
- Better quality
- Economy benefits to the planters
- Food vs fuel issue
- Increasing demands from the consumer products
The issue of using Fresh Edible Oil
Fresh Edible Oil
Oil Mill Effluent
Waste Cooking Oil
Fat
Waste Grease
Algae
Fresh non-edible oil
Low Quality Feedstock
World Biodiesel Congress & Expo;
December 05-07, 2016 San Antonio, Texas, USA.

5. Selection of catalyst Literature findings
Preparation of a sugar catalyst and its use for highly efficient production of biodiesel.
Min-Hua Zong,   Zhang-Qun Duan,   Wen-Yong Lou,  Thomas J. Smith and   Hong Wu  
Green Chem., 2007,9,
Feedstock: Waste cooking Oil
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

6. Incomplete carbonized char
Sugar Catalyst
Novel Preparation: Sulfonation of incomplete carbonized sugar
Sulphonation
Pyrolysis
Sugar
Incomplete carbonized char
Sugar catalyst
Green chemistry: Biodiesel made with sugar catalyst,
Toda et al., Nature 438, 178
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

7. Improved sugar catalyst?
(Sulfonated carbon catalyst)
Surface area (m2/g)
< 1
Total Acidity (mmol/g)
4.15
Pore Diameter (nm)
Undetected
Improved sugar catalyst?
Porous
High SA
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.
Jidon & Ellis, 2011,
Applied Catalysis A: general, 394, 25-31

8. Research Objectives
To increase the surface area and porosity of sugar catalyst
To characterize the improved sugar catalyst
To evaluate the catalytic activity on biodiesel production
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

9. Methodology Preparation of mesoporous char
Controlled functionalization via vapor phase sulfonation
Catalytic activity on esterification reaction (biodiesel synthesis)
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

10. Preparation of mesoporous char
D-glucose
P/Si
Pyrolysis
Char
Silica Removal
Mesoporous
char
Technique:
Confined Activation Process
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

11. Multiple vapour phase sulfonation
1. A heating mantle.
2. A round bottom flask.
3. A jacketed glass tube.
4. A heat exchanger.
5. A NaOH solution.
6. A silicon tube.
7. A vent line.
8. A thermometer.
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.
Experimental setup

12. Catalytic activity Batch Process
Reaction: Esterification of Oleic Acid with Methanol Reaction Conditions: Temp = 80OC (Reflux) Stirrer Speed = 800 rpm MeOH:OA MR = 10:1 Amount of catalyst = 3 wt% wrt OA
Batch Process
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

13. Results
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

14. Characterization Not as destructive as liquid sulfonation
Repeating the sulfonation step increases total acidity at the expense of surface area
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.
Fig. 3-7, pg. 41

15. Overall results
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

16. Conclusions
Mesoporous sugar catalyst could be produced by multiple vapour sulfonation of porous sugar char.
Multiple vapour phase sulfonation could increase total acidity at the expense of surface area.
The solid sugar catalyst had better catalytic activity on esterification reaction over the porous sugar catalyst, suggesting the reaction occurred on the surface of the catalyst and less likely inside the pores.
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.

17. Thank you for your attention!
World Biodiesel Congress & Expo; December 05-07, 2016 San Antonio, Texas, USA.