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In this study, the production of biodiesel from soybean oil by transesterification was carried out over sodium
aluminate as a heterogeneous catalyst. The solid base showed high catalytic activity for methanolysis reaching
a 93.9% yield under optimal reaction conditions (reflux temperature, 1.5 wt% of catalyst, 12:1 molar ratio of
methanol/oil, and 50 min). The catalyst treated at different temperatures was characterized by inductively
coupled plasma-optical emission spectroscopy (ICP-OES), X-ray diffraction (XRD), thermogravimetry/
differential thermogravimetry (TG/DTG), and Fourier transform infrared spectroscopy (FT-IR). The reaction
contained homogeneous and heterogeneous contributions at the same time. Removing water and carbon dioxide
was an effective way to elevate the catalyst stability in methanol.
Table 1. Operation Parameters for Spectro Genesis EOP Table 2. Basic Strengths, Solubility, and Catalytic Activities
ICP-OES with Different Calcination Temperatures of NaAlO2
RF generator power (W) 1400 basic solubilityb yieldc
frequency of RF generator (MHz) 27.12 thermal treatmenta strength (H_) (µg · mL-1) (%)
nebulizer type crossflow no 18 < H_ 120.7 89.9%
carrier gas flow rate (L min -1) 1 drying under infrared 15 < H_ <18 68.1 62.7%
coolant gas flow rate (L min -1) 14 light
auxiliary gas flow rate (L min -1) 1 200 °C 15 < H_ <18 127.8 83.0%
netto time (sec) 12 400 °C 15 < H_ <18 83.3 72.0%
analytical wavelength (nm) Na 589.592 600 °C 15 < H_ <18 81.6 66.2%
800 °C 9.8 < H_ <15 45.3 56.7%
600 °C used and recalcined not analyzed 40.0 62.9%
investigated its catalytic activity and the durability of soybean at 600 °C
oil to fatty acid methyl ester. a All thermal treatments were carried out for 4 h. b A 0.45 g quantity
Figure 5. Effect of methanol/oil molar ratio on the methyl ester yield. 4. Conclusions
Reaction condition: catalyst amount of 1.5%, reaction time of 30 min,
methanol reflux temperature. We aimed to investigate if SA was an effective heterogeneous
catalyst for biodiesel production. The solid base showed high
with carbon. The sharp absorption peaks at 610 cm-1, 560 cm-1, activity for the alcoholysis of soybean oil. The reaction was
and 490 cm-1 show the same component of aluminum species. carried out at a reflux temperature with a 12:1 molar ratio of
3.5. Catalytic Properties. The effects of reaction time, oil to methanol and 1.5% catalyst loading for a reaction time
methanol/oil molar ratio, and catalyst amount were studied. The varying from 10 to 60 min, in which the methyl ester yield
catalysts with no pretreatment were used in the catalysts’ reached 82.9-93.9%. In particular, catalytic durability tests
variables test. The influences of reaction time are illustrated in showed slight decrease in activity by repeating the transesteri-
Figure 4. The reaction rate for the initial 10 min was very fast fication reaction for three times.
and reached 93.9% at 50 min. The reason may partly be due to We also investigated the stability mechanism of SA. NaAlO2
the dissolution of the catalyst active species in methanol and adsorbed water and carbon dioxide, then changed the superficial
the formation of CH3O in the system. composition like NaAlO2 · χH2O and NaAl(OH)2CO3. They were
The influences of methanol/oil molar ratio are shown in easy to dissolve in methanol. At the same time, there was also
Figure 5. In heterogeneous catalysis, mass transfer and reactant probably a small part of NaAlO2 leaching into methanol.
adsorption on the catalyst is very important; thus, a molar ratio
higher than the stoichiometric molar ratio of methanol is needed Acknowledgment. The authors are grateful to Associate Profes-
to shift the equilibrium for the reaction. When the methanol/oil sor Man He in the centre of analysis and test of Wuhan University
molar ratio reached 15:1, the maximum conversion was for assistance with ICP tests.
obtained, which was distinguished from the value for the Supporting Information Available: Further details about the
homogeneous system.28 The production yield only improved a gas chromatography analysis are given in Figures S1 and S2.
little when the methanol/oil molar ratio was elevated from 12:1 This material is available free of charge via the Internet at
http://pubs.acs.org.
(28) Freedman, B.; Pryde, E. H.; Mounts, T. L. JAOCS 1984, 61, 1638–
1643. EF800904B