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Catalysts. A suite of catalysts were tested at 100 ̊C in methanol to assess their ability to transesterify triolein. Catalysts were chosen from literature [18, 20] representing effective catalysts for transesterification and inter- esterification and include basic, acidic, and neutral heterogeneous catalysts. The specific catalysts tested were Nafion, tungstosilicic acid hydrate, zeolites, CaO, K2CO3, hydrotalcite, and mesoporous silica (MCM-41). Yield is quantified based on mass balance and compared to positive controls (14% BF3 in methanol and H2SO4). Samples were treated similarly to standard transesterification using BF3. Results of the kinetics and yields of several chosen catalysts show that all of the tested catalysts achieve ~100% FAME yield within 4 hours with maximum yield occurring for basic catalysts within the first hour. The four catalysts, zeolite, hydrotalcite, MCM-41, and Nafion were chosen as representative basic, neutral, and acidic catalysts to continue experimentation. Upon implementation in the supercritical reaction, several factors will need to be considered for improved reaction yield including catalyst particle size and mixing speed to decrease mass transfer requirements. Phase Behavior. Experiments in a variable volume view cell indicated the phase behavior of the triglyceride, triolein, and its transesterification intermediates and products. These results show that while methanol increases the solubility of all of the substrates in CO2 that the relative solubilites are unchanged meaning that the FAME, methyl oleate, remains significantly more soluble than the rest of the substrates and that glycerol is still mostly insoluble. Interestingly the solubility of monoolein and diolein seemed to have increased more than triolein, meaning that despite their limited solubility in neat CO2, which could potentially cause reaction rate limitations, MG and DG solubility may not be an issue in the mixed system. CONCLUSIONS A More Optimal System: One-pot algal biodiesel production. Based on the current state of science and life cycle analyses, it is likely that a more optimal system for the production of algal biodiesel from a sustainability – economic, environmental, and social – perspective is a one-pot system using scCO2, methanol, and heterogeneous catalysts. Realization of this system requires enhanced understanding of the fundamental science determining the phase behavior and reactivity of each of the system components. The idealized system would efficiently extract TG from the biomass and facilitate transport to the catalyst for transesterification with the solubilized alcohol (Figure 6). The glycerol by-product would be insoluble and the FAME could be easily recovered from the SCF stream by decreasing temperature and pressure. This work has provided some of the foundations for realizing this system in terms of catalyst selection and understanding the fundamental phase behaviors to determine substrate and methanol loadings as well as reaction conditions. In order to make algae a viable industrial feedstock, the other unused biomass portions must be used efficiently in pursuit of a biorefinery model [48]. The biorefinery concept, in which both fuels and multiple value-added co- products are pursued in parallel [49] has been proposed as a way to assuage many of these concerns [50]. This point of view is promoted by the United States Department of Energy (DOE) National Algal Biofuels Technology Roadmap, which cites the potential for valuable co-products as one of the key reasons for exploring algae as a source of biofuels [51]. In our view, the biorefinery approach is both compelling and necessary. In the same way that petroleum refineries maximize profits and material efficiency through value optimization of every chemical fraction, so too must algal biorefineries if they are to be a viable and competitive alternative. In addition to economic considerations, the biorefinery concept is in accordance with the principles of green engineering [52] and a sustainable energy infrastructure. Figure 6: Depiction of possible reaction system configurationPDF Image | One-Pot Algal Biodiesel Production in Supercritical CO2
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