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Figure 2: Transesterification reaction Catalysts. In order to drive the reaction at minimal operating conditions, catalysts have been employed for transesterification. Alkaline, acidic, and enzymatic catalysts, homogeneous and heterogeneous, have all been explored for this application [17-22]. Homogeneous catalysts have been shown to work in all cases efficiently, but have significant barriers related to the contamination of the product and waste materials with these hazardous or expensive chemicals. Heterogeneous catalysts, however, can be easily recovered from the reaction and product mixture or embedded in a fixed bed for continuous operation and reuse [18]. Acidic and basic heterogeneous catalysts have been explored in a variety of solvents with varying degrees of success. Depending on the reaction conditions of temperature, alcohol: substrate ratio, catalyst loading, and time, as well as the catalyst properties of type, size, calcination/preparation time and temperature, up to a 96% conversion success of TG to FAME has been reported [18, 20]. The main downside to using heterogeneous catalysts is the decrease in efficiency in temperature requirements, yield, or kinetics. The application of supercritical fluids as the solvent for heterogeneously catalyzed transesterification can decrease this barrier as there is less resistance to mass transfer due to the decreased solvent viscosity [23]. Supercritical methanol (scMeOH) without a catalyst has also been used for triglyceride transesterification showing advantages in both system simplicity as well as reaction kinetics, but the higher operating temperature of at least 350 ̊C makes this option extremely energy intensive [24]. Despite the high temperature requirements, scMeOH may be the most energy efficient means to extract and convert lipid into biodiesel due to the decreased solvent and energy requirements for the single step process as well as the use of a wet algal feedstock [14]. While this technology has great potential, it still requires large amounts of energy to heat methanol past the supercritical point (239.1 ̊C) and is far from being commercially viable. Here we suggest using supercritical carbon dioxide with methanol as a co- solvent in order to produce a mixture that will be efficient at extraction, transesterification, and separation of products at much reduced operating temperatures, providing advantages seen through increased selectivity and solubility as well as decreased energy burden. Supercritical carbon dioxide (scCO2) has successfully been used commercially as a solvent for extraction, fractionation, and synthesis [25] with similar behavior to conventional solvents, hexane or ethyl acetate [26]. While it is not perfectly represented by either surrogate solvent, its properties allow it to efficiently and selectively extract non-polar compounds from complex matrices. There have been many studies [27-38] pertaining to lipid extraction by scCO2 in the food industry, particularly for nutrient removal from plants and algae. Of particular interest are long chain hydrocarbon compounds known to be soluble in scCO2 [30]. In algae, these products include valuable nutritive products such as carotenoids, chlorophylls, and ω3-fatty acids [28-32]. The effectiveness of lipid extraction from algae using scCO2 is explored in this work in terms of lipid yield and product selectivity. Further, scCO2’s selectivity offers a discrete advantage over conventional solvents during the conversion reaction in biodiesel. TG are moderately soluble while the FAME product is highly soluble (Figure 3) [39]. Compared to neat methanol where glycerol will not typically phase separate unless subjected to large drops in temperature or pressure [40, 41]), glycerol is almost insoluble in scCO2 and will precipitate out of solution upon formation. These disparate solubilities will potentially be favorable for driving the reaction equilibrium forward due to a relative decrease in product concentration.PDF Image | One-Pot Algal Biodiesel Production in Supercritical CO2
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