Name: Author Spotlight: Employing Green-Chemistry Principles for Safe and Sustainable Synthesis of Biodiesels
Uploaded: 2024-04-19T14:40:00
Description: Read this Scientific Article Protocol about Author Spotlight: Employing Green-Chemistry Principles for Safe and Sustainable Synthesis of Biodiesels at JoVE.com

The work was supported by Author YL&#39;s start-up fund and Pedagogy Enhancement Award (PEA) at California State University, Sacramento.

1. Oil source and preparation
<ol>
	<li>Add 2.0 mL of HPLC-grade methanol into a 15 mL centrifuge tube. 
	CAUTION: Methanol is a highly flammable liquid. It is toxic if swallowed, in contact with skin, or if inhaled, and it causes damage to the eyes. Ensure to wear personal protective equipment (PPE) when working with methanol and use it in the fume hood.</li>
	<li>Add one pellet of KOH (~0.10 g) to the centrifuge tube and dissolve the KOH solid using the ultrasonic cleaner (40 kHz) by just turnin...

Biodiesel Synthesis by Ultrasonic-Assisted Transesterification of Vegetable Oils

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P., Hamilton, A., Naccache, R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Biomass to bioenergy. , (2024).</li><li>Munir, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Biodiesel+production+from+novel+non-edible+caper+(Capparis+L.)+seeds+oil+employing+Cu-Ni+doped+ZrO2+catalyst.">Biodiesel production from novel non-edible caper (Capparis L.) seeds oil employing Cu-Ni doped ZrO2 catalyst.</a> Renew Sus Ener Rev. 138, 110558 (2021).</li><li>Munir, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cleaner+production+of+biodiesel+from+novel+non-edible+seed+oil+(Carthamus+lanatus+L.)+via+highly+reactive+and+recyclable+green+nano+CoWO3@rGO+composite+in+context+of+green+energy+adaptation.">Cleaner production of biodiesel from novel non-edible seed oil (Carthamus lanatus L.) via highly reactive and recyclable green nano CoWO3@rGO composite in context of green energy adaptation.</a> Fuel. 332, 126265 (2023).</li><li>Rocha-Meneses, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recent+advances+on+biodiesel+production+from+waste+cooking+oil+(WCO):+A+review+of+reactors,+catalysts,+and+optimization+techniques+impacting+the+production.">Recent advances on biodiesel production from waste cooking oil (WCO): A review of reactors, catalysts, and optimization techniques impacting the production.</a> Fuel. 348, 128514 (2023).</li><li>Suslick, K. 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A., Wang, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ultrasonic-assisted+synthesis,+characterization,+and+application+of+a+metal-organic+framework:+A+green+general+chemistry+laboratory+project.">Ultrasonic-assisted synthesis, characterization, and application of a metal-organic framework: A green general chemistry laboratory project.</a> J Chem Edu. 96 (10), 2286-2291 (2019).</li><li>Tan, S. X., Lim, S., Ong, H. C., Pang, Y. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=State+of+the+art+review+on+development+of+ultrasound-assisted+catalytic+transesterification+process+for+biodiesel+production.">State of the art review on development of ultrasound-assisted catalytic transesterification process for biodiesel production.</a> Fuel. 235, 886-907 (2019).</li><li>Mahamuni, N. N., Adewuyi, Y. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fourier+transform+infrared+spectroscopy+(FTIR)+method+to+monitor+soy+biodiesel+and+soybean+oil+in+transesterification+reactions,+petrodiesel&#8722;+biodiesel+blends,+and+blend+adulteration+with+soy+oil.">Fourier transform infrared spectroscopy (FTIR) method to monitor soy biodiesel and soybean oil in transesterification reactions, petrodiesel&#8722; biodiesel blends, and blend adulteration with soy oil.</a> Ener Fuels. 23 (7), 3773-3782 (2009).</li><li>Castej&#243;n, D., Fricke, P., Cambero, M. I., Herrera, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Automatic+1H-NMR+screening+of+fatty+acid+composition+in+edible+oils.">Automatic 1H-NMR screening of fatty acid composition in edible oils.</a> Nutrients. 8 (2), 93 (2016).</li><li>Doudin, K. I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Quantitative+and+qualitative+analysis+of+biodiesel+by+NMR+spectroscopic+methods.">Quantitative and qualitative analysis of biodiesel by NMR spectroscopic methods.</a> Fuel. 284, 119114 (2021).</li><li>Prat, D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chem21+selection+guide+of+classical-and+less+classical-solvents.">Chem21 selection guide of classical-and less classical-solvents.</a> Green Chem. 18 (1), 288-296 (2016).</li><li>Ameen, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Prospects+of+catalysis+for+process+sustainability+of+eco-green+biodiesel+synthesis+via+transesterification:+A+state-of-the-art+review.">Prospects of catalysis for process sustainability of eco-green biodiesel synthesis via transesterification: A state-of-the-art review.</a> Sustainability. 14 (12), 7032 (2022).</li><li>Malek, M. N. F. A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ultrasonication:+A+process+intensification+tool+for+methyl+ester+synthesis:+A+mini+review.">Ultrasonication: A process intensification tool for methyl ester synthesis: A mini review.</a> Biomass Conv Bioref. 13, 1457-1467 (2023).</li></ol>

In this demonstration, an ultrasonic assisted method of base-catalyzed production of biodiesel is elucidated for optimal efficacy. For optimal results, the centrifuge tube should be placed inside a beaker filled with water and then the beaker should be placed within the ultrasonic bath. This immersed configuration guarantees thorough exposure of the reaction mixture to the ultrasonic treatment, maximizing its effectiveness. If desired, a centrifuge rack can also be used to replace the beaker inside the ultrasonic bath, w...

Biodiesel, derived from common, plant-based oils and fats, emerges as a sustainable solution to mitigate reliance on petroleum1. This renewable substitute showcases reduced greenhouse gas emissions, notably carbon dioxide, while relying on sustainable resources. Furthermore, biodiesel presents distinct advantages over petroleum diesel, characterized by its sulfur-free composition, non-toxic nature, and biodegradability. As an alternative to conventional fossil fuels, biodiesel aligns with the United Nations&#39; (UN&#39;s) Net Zero policy by reducing our dependence on non-renewable fossil fuels and mitigating the adverse effects of climate change. Biodiesel offers a promising path to meeting current energy needs, making it a powerful choice for a greener future2.
The predominant method used for biodiesel production involves transesterification, a chemical process where triglycerides found in oils and fats react with an alcohol, typically methanol or ethanol, in the presence of a catalyst under elevated temperature conditions1,2,3,4.&#160;This reaction yields fatty acid alkyl esters, the principal component of biodiesel. Various types of vegetable oils serve as primary feedstocks for biodiesel production, including both edible5 (e.g., extra virgin olive oil and corn oil) and non-edible oils6,7,8 (e.g., caper seed oil), as well as waste oils9. Methanol is most commonly used for this transesterification process as it is a relatively inexpensive alcohol. Additionally, an array of catalysts such as sulfuric acid, phosphoric acid, potassium hydroxide, sodium hydroxide, or enzymes like lipase can be used to expedite the transesterification process1,2,3,4. Traditionally, the reaction mixture is heated under reflux for prolonged periods, typically 30 min or more. Heating is not as energy efficient as ultrasonication while also posing safety risks5. Consequently, there is a need for a safer, faster, and more energy efficient transesterification process.
Ultrasound irradiation emerges as a superior alternative to conventional energy sources such as heat, light, and electricity, primarily due to the phenomenon of acoustic cavitation10. This phenomenon, characterized by the formation, expansion, and violent collapse of bubbles, generating localized hotspots with temperatures reaching approximately 5000 K and pressures of 1000 atm. Such extreme conditions, coupled with rapid heating and cooling rates (over 1010 K/s), furnish the requisite energy for a wide array of chemical reactions to occur efficiently at room temperature, including those previously deemed unattainable by conventional means10. Ultrasonic-assisted synthesis is rapidly gaining ground across diverse research areas. Notably, interest in ultrasonic-assisted synthesis in organic synthesis and solid-state materials is driven by its environmentally friendly nature, energy efficiency, and abbreviated reaction times under ambient conditions5,11,12,13,14,15,16.&#160;A prompt and effective technique is introduced here for secure ultrasonic-assisted transesterification of vegetable oils using an alkaline catalyst yielding pure biodiesel products within a short time frame. While extra virgin olive oil serves as the demonstration medium in this study, it is imperative to note that the ultrasonic method holds applicability to a spectrum of vegetables oils5,17.

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>Chloroform-d</td>
			<td>Fisher Scientific</td>
			<td>865-49-6</td>
			<td>&#8226; Harmful if swallowed. 
			&#8226; Causes skin irritation. 
			&#8226; Causes serious eye irritation. 
			&#8226; Toxic if inhaled. 
			&#8226; Suspected of causing cancer. 
			&#8226; Suspected of damaging fertility or the unborn child. 
			&#8226; Causes damage to organs through prolonged or repeated exposure</td>
		</tr>
		<tr>
			<td>Heated Ultrasonic Baths, Digital, Branson Ultrasonic</td>
			<td>Branson&#160;</td>
			<td>89375-492</td>
			<td></td>
		</tr>
		<tr>
			<td>Methanol</td>
			<td>Fisher Scientific Company</td>
			<td>67-56-1</td>
			<td>Highly flammable liquid and vapor. Toxic if swallowed, in contact with skin or if inhaled. Causes damage to organs (Eyes).</td>
		</tr>
		<tr>
			<td>Potassium hydroxide&#160;</td>
			<td>Fisher Scientific Company</td>
			<td>1310-58-3</td>
			<td>May be corrosive to metals. Harmful if swallowed. Causes severe skin burns and eye damage. Causes serious eye damage</td>
		</tr>
		<tr>
			<td>Sodium chloride</td>
			<td>Sigma-Aldrich</td>
			<td>7647-14-5</td>
			<td>Not hazardous</td>
		</tr>
		<tr>
			<td>Vegetable oils</td>
			<td></td>
			<td></td>
			<td>A commonly consumed food with a long history of safe use in pesticides.&#160;</td>
		</tr>
	</tbody>
</table>

ultrasonic-assisted preparation of biodiesel products from vegetable oils

Utilizing vegetable oil as a sustainable feedstock, this study presents an innovative approach to ultrasonic-assisted transesterification for biodiesel synthesis. This alkaline-catalyzed procedure harnesses ultrasound as a potent energy input, facilitating the rapid conversion of extra virgin olive oil into biodiesel. In this demonstration, the reaction is run in an ultrasonic bath under ambient conditions for 15 min, requiring a 1:6 molar ratio of extra virgin olive oil to methanol and a minimum amount of KOH as the catalyst. The physiochemical properties of biodiesel are also reported. Emphasizing the remarkable advantages of ultrasonic-assisted transesterification, this method demonstrates notable reductions in reaction and separation times, achieving near-perfect purity (~100%), high yields, and negligible waste generation. Importantly, these benefits are achieved within a framework that prioritizes safety and environmental sustainability. These compelling findings underscore the effectiveness of this approach in converting vegetable oil into biodiesel, positioning it as a viable option for both research and practical applications.

Author Spotlight: Employing Green-Chemistry Principles for Safe and Sustainable Synthesis of Biodiesels

Ultrasonic-Assisted Preparation of Biodiesel Products from Vegetable Oils

In this demonstration, the transesterification reaction of extra virgin olive oil and methanol, catalyzed by KOH, produces biodiesel at room temperature in an ultrasonic bath (Figure 1)5. The starting materials in the centrifuge tube show the reactants are immiscible and divided into two layers as seen in Figure 2A. The upper layer is a mixture of methanol and KOH while the lower layer is composed of extra virgin olive oil. To promote hom...

Read this Scientific Article Protocol about Author Spotlight: Employing Green-Chemistry Principles for Safe and Sustainable Synthesis of Biodiesels at JoVE.com

A safe ultrasonic-assisted transesterification method for vegetable oils using an alkaline catalyst is presented here. The method is rapid and efficient for preparing pure biodiesel products.

Utilizing vegetable oil as a sustainable feedstock, this study presents an innovative approach to ultrasonic-assisted transesterification for biodiesel ...