This work investigates the catalytic activity of geopolymers produced using two different alkali components (sodium or potassium) and four treatment temperatures (110 to 700 °C) for the methyl transesterification of soybean oil. The geopolymers were prepared with metakaolin as an aluminosilicate source and alkaline activating solutions containing either sodium or potassium in the same molar oxide proportions. The potassium-based formulation displayed a higher specific surface area and lower average pore size (28.64–62.54 m²/g; 9 nm) than the sodium formulation (6.34–32.62 m²/g; 17 nm). The reduction in specific surface area (SSA) after the heat treatment was more severe for the sodium formulation due to the higher thermal shrinkage. The catalytic activity of the geopolymer powders was compared under the same reactional conditions (70–75 °C, 150% methanol excess, 4 h reaction) and same weight amounts (3% to oil). The differences in performance were attributed to the influences of sodium and potassium on the geopolymerization process and to the accessibility of the reactants to the catalytic sites. The Na-based geopolymers performed better, with FAME contents in the biodiesel phase of 85.1% and 89.9% for samples treated at 500 and 300 °C, respectively. These results are competitive in comparison with most heterogeneous base catalysts reported in the literature, considering the very mild conditions of temperature, excess methanol and catalyst amount and the short time spent in reactions.
SiO2-SO3H, with a surface area of 115 m2·g−1, pore volumes of 0.38 cm3·g−1 and 1.32 mmol H+/g, was used as a transesterification catalyst. Triglycerides of waste cooking oil reacted with methanol in refluxing toluene to yield mixtures of diglycerides, monoglycerides and fatty acid methyl esters (FAMEs) in the presence of 20% (w/w) catalyst/oil using the hydrophilic sulfonated silica (SiO2-SO3H) catalyst alone or with the addition of 10% (w/w) co-catalyst/oil [(Bun4N)(BF4) or Aliquat 336]. The addition of the ammonium salts to the catalyst lead to a decrease in the amounts of diglycerides in the products, but the concentrations of monoglycerides increased. Mixtures of (Bun4N)(BF4)/catalyst were superior to catalyst alone or Aliquat 336/catalyst for promoting the production of mixtures with high concentrations of FAMEs. The same experiments were repeated using DMSO as the solvent. The use of the more polar solvent resulted in excellent conversion of the triglycerides to FAME esters with all three-catalyst media. A simplified mechanism is presented to account for the experimental results.
Hydroesterification is innovation biodiesel production using low cost feedstock by two-step: hydrolysis of waste cooking oil to FFAs in subcritical water and chemical esterification of FFAs into FAME (biodiesel) with methanol. The purpose was to apply the experimental factorial design to evaluate the influence of reaction variables on the effectiveness of hydrolysis and determine the relationship of FFAs and FAMEs yields. Experiments were conducted in a batch reactor under diverse reaction conditions to determine the optimal parameters for hydrolysis. This analyses indicated that high FFAs yields (95 wt%) are achieved using 250 C; 120 min; 100:1 water-to-oil molar ratio and 700 rpm. Research results revealed a conversion the FFAs in 98.5 wt% of FAMEs with high quality by esterification in biodiesel production. This study shows that the biodiesel produced by subcritical/chemical hydroesterification process has similar qualities to the biodiesel obtained by traditional alkaline transesterification, which suggests a promising alternative for biodiesel production.
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