Synthesis, Characterization and Evaluation of Sulphated Zirconias for Biodiesel Production by Triglyceride Cracking

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1 Synthesis, Characterization and Evaluation of Sulphated Zirconias for Biodiesel Production by Triglyceride Cracking Elizabeth J. Eterigho, J. G. M. Lee & A. P. Harvey School of Chemical Engineering and Advanced Materials Newcastle University, UK Bioenergy III: Present and New Perspectives on Biorefineries Lanzarote, May, 2011

2 utline Introduction Motivation of study bjective Experimental Results Conclusions

3 Introduction Biodiesel are mono-alkyl esters of fatty acids derived from natural oils. (FAMEs) renewable, Carbon neutral i. e. Not adding to the global warming crisis it is sustainable Conventional method Introduction Motivation bjective Experimental Results Conclusions

4 Motivation European Directive of 2009/28/EC, proposed 10% renewable fuel by the end of ~ 35 mtoe biofuel (i.e. 22 mtoe biodiesel &13 mtoe bioethanol) Source of data : Renewable Energy Association Global transport fuel demand is set to rise by 45% in Source of data: Shell calculations based on IEA and PIRA data Neste oil, (2008) Introduction Motivation bjective Experimental Results Conclusions

5 Transesterification Process 15% MeH X il Thermo Transesterifica catalytic cracking tion MeH Recovery 66% Washing 11% FAME purifica tion FAMEs Solid NaH acid catalyst X Catalyst NaH Catalyst removal Glycerol removal X Glycerol Introduction Motivation bjective Experimental Results Conclusions

6 Sulphated zirconia S Z r Sulphated zirconia is: super-acid catalyst with acidity 10 4 times stronger than 100% sulphuric acid good for organic reactions + Z r H Z r S Z r Drawbacks: a relatively small surface area rapid deactivation and sulphate leaching, Introduction Motivation bjective Experimental Results Conclusions

7 bjective The main objective of our research is to improve the catalytic activity of sulphated zirconia for high activity and selectivity towards desired products. Two different methods of Preparation Direct method (ds), simple calcination of ZrCl 2.8H 2 and (NH 4 ) 2 S 4 for 5 hours at 600 o C Conventional method (cm) ZrCl 2.8H 2 was hydrolysed with NH 4 H, Zr(H) 4 was impregnated with H 2 S 4 Calcination for 3 hours at 650 o C. Characterization of catalysts Introduction Motivation bjective Experimental Results Conclusions

8 Catalyst synthesis Conventional method cm NH 4 H ZrCl 2.8H 2 H 2 S 4 H 2 hydrolysis filtration drying sulphating drying calcination S/Zr H 2 H 2 S 4 (NH 4 ) 2 S4 ZrCl 2.8H 2 Direct method ds mixing calcination S/Zr Introduction Motivation bjective Experimental Results Conclusions

9 Catalyst application S/Zr Gases TG Catalytic Cracking Analysis of liquid sample Light olefins Light paraffins Biodiesel Alcohol Aromatics Introduction Motivation bjective Experimental Results Conclusions

10 Characterization results c m d s lntensity M T T M T th e ta th e ta XRD of cm and ds catalysts Introduction Motivation bjective Experimental Results Conclusions

11 Characterization results 70 DS Absorbance (%) L B = Bronsted site L = Lewis site 1s cm 45 B cm 1s ds 64 Absorbance (%) B L Binding energy (ev) XPS results for xygen on the surface of the catalysts IR spectra of adsorbed pyridine on the catalysts Introduction Motivation bjective Experimental Results Conclusions

12 Characterization results 50 ds cm 180 Properties DS CM BET surface area FAMEs (%) Surfa ace area (m 2 /g) (m 2 /g) Pore size (µm) Particle size (µm) Sulphate content in sulphating agent (wt% ) Effect of SA and S 4 2- /loading on biodiesel (FAMEs) production Crystallite size (nm) Nature of phases A T, M Introduction Motivation bjective Experimental Results Conclusions

13 Results 40 Saturated Unsaturated Mass conc centration (%) cm ds FAMEs (mass %) FAMEs (mass %) Time (min) Time (min) Saturated Unsaturated Reaction tim e (m in) Introduction Motivation bjective Experimental Results Conclusions

14 Results 80 C18:1 70 cm ds 60 C16 Selectivity of the catalysts Mass of FA AMEs (%) C14 C18 C18:2 C18:3 >C18: m yristate palm itate stearate oleate linoleate linolenate others Type of FAMEs FAMEs profile showing saturated, mono and poly unsaturated Introduction Motivation bjective Experimental Results Conclusions

15 Summary Catalyst type Conversion BET surface area (m 2 /g) Pore size (µm) Particle size (µm) Crystallite size (nm) Nature of phases FAMEs (%) Acid sites (%) B L DS A CM T, M Introduction Motivation bjective Experimental Results Conclusions

16 Conclusions Both catalysts were active and contain ``Bronsted sites and Lewis sites. The morphology of ds contributed to it higher activity Both catalysts were selective but ds exhibited higher selectivity, ~ 50% for FAMEs However the cm exhibited a unique selectivity for saturated fatty acid methyl esters verall The preparation method showed improved physical and chemical properties of the catalysts which influenced their activity observed in the yield of fatty acid methyl ester. Biodiesel (FAMEs) can be produced by thermocatalytic cracking of triglycerides using these catalyst from both method of preparation. Introduction Motivation bjective Experimental Results Conclusions

17 Future work Further improvement of the catalysts, for optimization of performance and more selectivity. The use of non-edible feedstock Introduction Motivation bjective Experimental Results Future work

18 Acknowledgements Thanks to the following for their contributions: Dr A. P. Harvey Dr J. G. M. Lee Karen Wilson; Cardiff University Petroleum Trust Development Fund Introduction Motivation bjective Experimental Results Acknowledgements

19 THANKS FR LISTENING Bioenergy III May 22 27, 2011

20 Mechanism C H 2 C R C H C R ca ta lyst h ig h te m p. R C H + R C H C + C H 2 C C H C H 2 C R R C H C ; C H 2 C C H ca ta ly st cra ck in g C a rb o xylic a cid s + H y d ro ca rb o n s + E ste rs C 2 + C n H 2 n + 2 R C H C + H 2 + C nh 2 n First is deoxygenation by thermal cracking followed by catalytic cracking, oligomerization, alkylation etc of triglycerides Suarez, P. A. Z. (2006) thermo- catalytic cracking of triglycerides (

21 100 H 55 Alcohol 2-cis-9-0ctadecenyloxy ethanol ) E-14-Hexadecenal H ) 1-Heptatriacotanol

22 Evidence of catalytic cracking 2.50E+009 RS il 2.00E+009 cm 1.50E E+009 Abundance 5.00E E E E E+010 ds 1.00E E+009 thermal 6.00E E E E E Time (min) Introduction Motivation bjective Experimental Results Conclusions

23 % Transmittance Catalysts leaching 102 CM (used) CM (unused) % Transmittance 96 DS (used) 90 DS (unused) wave number (cm-1)

24 Vegetable il + catalyst Deoxygenation and cracking Condensation Heavy hydrocarbons +xygenates Coke Polymerization Deoxygenation and secondary cracking Light olefins + light paraffins (gasoline) + C 2 +alcohol +C +H 2 ligomerization Aromatic Hydrocarbons Alkylation, Isomerization and Aromatization lefins + paraffins (gasoline, biodiesel and kerosene) Gases (light olefins, paraffins, C, C 2 + H 2 )

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