Catalytic Esterification of Levulinic Acid to Alkyl Levulinates: Liquid Product Analysis and Separation Study via Extraction

The present work unlocks the full potential of sulfonated lignin-based carbon (SLBC) catalyst in the esterification of levulinic acid (LA) with different alcohols such as methanol, ethanol, and n-butanol to alkyl levulinates (ALs), followed by liquid product analysis and product separation. Lignin w...

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Main Authors: Abdull Hafidz Hassan, Muzakkir Mohammad Zainol, Mohammad Zakwan Zainol, Mohd Asmadi, Mohd Yazid Yusof
Format: Article
Language:English
Published: AIDIC Servizi S.r.l. 2024-11-01
Series:Chemical Engineering Transactions
Online Access:https://www.cetjournal.it/index.php/cet/article/view/14810
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author Abdull Hafidz Hassan
Muzakkir Mohammad Zainol
Mohammad Zakwan Zainol
Mohd Asmadi
Mohd Yazid Yusof
author_facet Abdull Hafidz Hassan
Muzakkir Mohammad Zainol
Mohammad Zakwan Zainol
Mohd Asmadi
Mohd Yazid Yusof
author_sort Abdull Hafidz Hassan
collection DOAJ
description The present work unlocks the full potential of sulfonated lignin-based carbon (SLBC) catalyst in the esterification of levulinic acid (LA) with different alcohols such as methanol, ethanol, and n-butanol to alkyl levulinates (ALs), followed by liquid product analysis and product separation. Lignin was calcined to produce carbon material, modified into the SCLB catalyst by hydrothermal sulfonation, and finally characterized. The reaction was performed over SLBC catalyst in selected reaction conditions of 6 molar ratio of alcohol-to-LA, 0.3 g catalyst, and 5 h at respective alcohol reflux temperatures. The liquid products were examined by acid-base titration and then quantified using gas chromatography coupled with mass spectrometry (GC-MS) for comparison of data. The separation of the synthesized ALs and simulated ALs-LA mixture was conducted via liquid-liquid extraction, utilizing 9:1 hexane-water (v/v) mixture as the extraction solvent. The SLBC catalyst successfully yielded ALs (methyl, ethyl, and butyl levulinates) of 73.5–83.3 mol%. The hexane-water mixture was able to extract ALs from the liquid mixtures and the percentage extraction increased for longer alkyl chains of ALs. The acid-base titration demonstrated a minimal percentage difference with GC-MS data for LA conversion and could be suggested as a reliable liquid product analysis, especially for LA esterification reaction.
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institution Kabale University
issn 2283-9216
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publishDate 2024-11-01
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record_format Article
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spelling doaj-art-62bd55c97bc344e1a94c8281caec1ff62024-12-01T00:38:26ZengAIDIC Servizi S.r.l.Chemical Engineering Transactions2283-92162024-11-01113Catalytic Esterification of Levulinic Acid to Alkyl Levulinates: Liquid Product Analysis and Separation Study via ExtractionAbdull Hafidz HassanMuzakkir Mohammad ZainolMohammad Zakwan ZainolMohd Asmadi Mohd Yazid YusofThe present work unlocks the full potential of sulfonated lignin-based carbon (SLBC) catalyst in the esterification of levulinic acid (LA) with different alcohols such as methanol, ethanol, and n-butanol to alkyl levulinates (ALs), followed by liquid product analysis and product separation. Lignin was calcined to produce carbon material, modified into the SCLB catalyst by hydrothermal sulfonation, and finally characterized. The reaction was performed over SLBC catalyst in selected reaction conditions of 6 molar ratio of alcohol-to-LA, 0.3 g catalyst, and 5 h at respective alcohol reflux temperatures. The liquid products were examined by acid-base titration and then quantified using gas chromatography coupled with mass spectrometry (GC-MS) for comparison of data. The separation of the synthesized ALs and simulated ALs-LA mixture was conducted via liquid-liquid extraction, utilizing 9:1 hexane-water (v/v) mixture as the extraction solvent. The SLBC catalyst successfully yielded ALs (methyl, ethyl, and butyl levulinates) of 73.5–83.3 mol%. The hexane-water mixture was able to extract ALs from the liquid mixtures and the percentage extraction increased for longer alkyl chains of ALs. The acid-base titration demonstrated a minimal percentage difference with GC-MS data for LA conversion and could be suggested as a reliable liquid product analysis, especially for LA esterification reaction.https://www.cetjournal.it/index.php/cet/article/view/14810
spellingShingle Abdull Hafidz Hassan
Muzakkir Mohammad Zainol
Mohammad Zakwan Zainol
Mohd Asmadi
Mohd Yazid Yusof
Catalytic Esterification of Levulinic Acid to Alkyl Levulinates: Liquid Product Analysis and Separation Study via Extraction
Chemical Engineering Transactions
title Catalytic Esterification of Levulinic Acid to Alkyl Levulinates: Liquid Product Analysis and Separation Study via Extraction
title_full Catalytic Esterification of Levulinic Acid to Alkyl Levulinates: Liquid Product Analysis and Separation Study via Extraction
title_fullStr Catalytic Esterification of Levulinic Acid to Alkyl Levulinates: Liquid Product Analysis and Separation Study via Extraction
title_full_unstemmed Catalytic Esterification of Levulinic Acid to Alkyl Levulinates: Liquid Product Analysis and Separation Study via Extraction
title_short Catalytic Esterification of Levulinic Acid to Alkyl Levulinates: Liquid Product Analysis and Separation Study via Extraction
title_sort catalytic esterification of levulinic acid to alkyl levulinates liquid product analysis and separation study via extraction
url https://www.cetjournal.it/index.php/cet/article/view/14810
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AT muzakkirmohammadzainol catalyticesterificationoflevulinicacidtoalkyllevulinatesliquidproductanalysisandseparationstudyviaextraction
AT mohammadzakwanzainol catalyticesterificationoflevulinicacidtoalkyllevulinatesliquidproductanalysisandseparationstudyviaextraction
AT mohdasmadi catalyticesterificationoflevulinicacidtoalkyllevulinatesliquidproductanalysisandseparationstudyviaextraction
AT mohdyazidyusof catalyticesterificationoflevulinicacidtoalkyllevulinatesliquidproductanalysisandseparationstudyviaextraction