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Ultrasound-assisted solid Lewis acid-catalyzed transesterification of Lesquerella fendleri oil for biodiesel synthesis.

ABSTRACT: Biodiesel, a mixture of fatty acid methyl esters (FAME), is bio-renewable, non-toxic, biodegradable, and is an attractive alternative to petroleum diesel. This work studied the sonochemical transesterification of Lesquerella fendleri oil (LFO) using inexpensive solid Lewis acid (LA) catalysts with an aim to reduce environmental pollution and dependance on non-renewable fuel sources. Due to the presence of hydroxy fatty acid methyl esters (HFAME) in LFO (∼60%), in addition to producing biofuel it can also be used to generate chemically important estolides and cyclic lactones. AlCl₃, SnCl₂, and Sn(CH₃COO)₂ showed catalytic activity using direct immersion ultrasound (DI-US) among a list of LA catalysts investigated, with AlCl₃ being the best catalyst. Ultrasound increased the reaction rate by facilitating carbocation formation of glyceridic carbons. Experiments were carried out at room temperature in a solvent range from 3:1 to 18:1 methanol-to-oil molar ratio and catalyst loading from 1 wt% to 6 wt% over 10 to 60 min sonication time at 48% ultrasound amplitude (roughly 17 W/cm²). Complete conversion (>99%) was achieved in 40 min with 5 wt% AlCl₃ catalyst. A statistical regression analysis with STATA 14.0 software was performed to optimize process parameters. Chemical characterizations of the compounds were performed with nuclear magnetic resonance (NMR) spectroscopy (¹H NMR & ¹³C NMR), and % conversion of FAMEs was calculated from the ¹H NMR spectra. The fatty acid profile was determined by GC-FID and GC-MS analysis. FT-IR spectroscopic analysis and thermogravimetric analysis (TGA) were performed to investigate the infrared absorption pattern of the compound and the volatility difference between Lesquerella fendleri biodiesel and oil under nitrogen atmosphere. Results indicate that this is a fast, green, energy-efficient, sustainable, and industrially applicable method for biodiesel production from LFO.

SUBMITTER: Shahidul Islam M

PROVIDER: S-EPMC9256648 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Project description:To produce biodiesel cost-effective, low-cost, high free fatty acid (FFA) oil feedstock is desirable. But high FFA creates difficulty during the base-catalyzed transesterification process by yield loss due to the formation of soap. However, these problems are overcome by the use of an acid catalyst. The acid catalysts can directly convert both triglycerides and FFAs into biodiesel without the formation of soaps or emulsions. The shortcomings of mostly used inorganic acids are that they work well for esterification of FFA present in low-cost oil, but their kinetics for transesterification of triglycerides present in oils is considerably slower. Corrosion of equipment is another major problem associated with an inorganic acid catalyst. The usage of an organic acid catalyst of the alkyl benzene sulfonic type, like 4-dodecyl benzene sulfonic acid (DBSA) minimizes these disadvantages of inorganic acid-catalyzed transesterification. The aim of the present investigation was to reduce the reaction time of transesterification of triglycerides further by using microwaves as a heating source in the presence of DBSA catalyst to achieve higher conversions under mild operating conditions. To optimize the transesterification variables for the higher conversion of biodiesel, the response surface methodology was employed to design the experiment. By using the DBSA catalyst under microwave heating at a temperature of 76 °C, conversion close to 100% in only 30 min of reaction time was obtained using a 0.09 molar ratio of catalyst to oil and 9.0 molar ratio of methanol to oil. A modified polynomial model was developed and was adequately fitted with the experimental data and could be used for understanding the effect of various process parameters. The catalyst to oil molar ratio and reaction temperature created a stronger effect on the biodiesel production than that exhibited by the methanol to oil molar ratio. It was observed that the microwave heating process outperformed conventional heating, providing a rapid, easy method for biodiesel synthesis from triglycerides in the presence of DBSA, an organic acid catalyst. The produced biodiesel was of good quality, as all the properties were within the prescribed limits of the ASTM D6751 standard.

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Ultrasound-assisted solid Lewis acid-catalyzed transesterification of Lesquerella fendleri oil for biodiesel synthesis.

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