Cornejo Ibergallartu, Alfonso
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Cornejo Ibergallartu
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Alfonso
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InaMat2. Instituto de Investigación en Materiales Avanzados y Matemáticas
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Publication Open Access Bio-oil fractionation according to polarity and molecular size: characterization and application as antioxidants(American Chemical Society, 2024-12-21) Fonts, Isabel; Lázaro, Cristina; Cornejo Ibergallartu, Alfonso; Sánchez, José Luis; Afailal, Zainab; Gil-Lalaguna, Noemí; Arauzo, Jesús María; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Gobierno de Navarra / Nafarroako GobernuaBio-oil obtained from biomass pyrolysis has great potential for several applications after being upgraded and refined. This study established a method for separating bio-oil into different fractions based on polarity and molecular size to extract phenolic and polyphenolic compounds with antioxidant properties. The fractions were analyzed using various spectroscopic and chromatographic techniques, such as GC/MS, FTIR, UV-vis, SEC, DOSY-NMR, 13C-NMR, and 31P-NMR. The antioxidant properties of these fractions were tested by examining their ability to improve the oxidative stability of biodiesel. The results strongly connected the bio-oil's chemical functionalities and antioxidant power. During solvent fractionation, dichloromethane could extract phenolic structures, which were subsequently size-fractionated. The subfractions with lower molecular weight (in the order of monomers and dimers) outperformed the antioxidant potential of the crude bio-oil. Heavier subfractions from dichloromethane extraction did not show good antioxidant abilities, which was related to the low hydroxy group content. After solvent extraction, phenolic oligomers remained in the water-insoluble/dichloromethane-insoluble fraction, which showed good antioxidant potential despite its low solubility in biodiesel.Publication Open Access Exploring a low-cost valorization route for amazonian cocoa pod husks through thermochemical and catalytic upgrading of pyrolysis vapors(American Chemical Society, 2023) Villasana, Yanet; Armenise, Sabino; Ábrego, Javier; Hablich, Karina; Bimbela Serrano, Fernando; Cornejo Ibergallartu, Alfonso; Gandía Pascual, Luis; Ciencias; Zientziak; Institute for Advanced Materials and Mathematics - INAMAT2; Universidad Pública de Navarra / Nafarroako Unibertsitate PublikoaEcuador as an international leader in the production of cocoa beans produced more than 300 000 tons in 2021; hence, the management and valorization of the 2 MM tons of waste generated annually by this industry have a strategic and socioeconomic value. Consequently, appropriate technologies to avoid environmental problems and promote sustainable development and the bioeconomy, especially considering that this is a megadiverse country, are of the utmost relevance. For this reason, we explored a low-cost pyrolysis route for valorizing cocoa pod husks from Ecuador’s Amazonian region, aiming at producing pyrolysis liquids (bio-oil), biochar, and gas as an alternative chemical source from cocoa residues in the absence of hydrogen. Downstream catalytic processing of hot pyrolysis vapors using Mo- and/or Ni-based catalysts and standalone γ-Al2O3 was applied for obtaining upgraded bio-oils in a laboratory-scale fixed bed reactor, at 500 °C in a N2 atmosphere. As a result, bimetallic catalysts increased the bio-oil aqueous phase yield by 6.6%, at the expense of the organic phase due to cracking reactions according to nuclear magnetic resonance (NMR) and gas chromatography–mass spectrometry (GC–MS) results. Overall product yield remained constant, in comparison to pyrolysis without any downstream catalytic treatment (bio-oil ∼39.0–40.0 wt % and permanent gases 24.6–26.6 wt %). Ex situ reduced and passivated MoNi/γ-Al2O3 led to the lowest organic phase and highest aqueous phase yields. The product distribution between the two liquid phases was also modified by the catalytic upgrading experiments carried out, according to heteronuclear single-quantum correlation (HSQC), total correlation spectroscopy (TOCSY), and NMR analyses. The detailed composition distribution reported here shows the chemical production potential of this residue and serves as a starting point for subsequent valorizing technologies and/or processes in the food and nonfood industry beneficiating society, environment, economy, and research.