Faculty Publications
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Item Straightforward synthesis of calcium levulinate from biomass-derived levulinic acid and calcium carbonate in egg-shells(Elsevier Ltd, 2019) Sharath, B.O.; Tiwari, R.; Mal, S.S.; Dutta, S.Calcium levulinate (CL) is a nutritional supplement for calcium and a chemical intermediate in synthesizing levulinic biofuels. The reported synthesis of CL involve reaction between cellulose-derived levulinic acid (LA) and calcium hydroxide in an aqueous medium. In this work, we report the production of CL using CaCO3 from poultry egg shells. The scalable production uses biomass-derived LA and egg-shell derived CaCO3 under conventional heating and mechanical stirring. The reaction was optimized on temperature, duration of reaction, and equivalent of CaCO3. Using 1.5 equivalent of CaCO3, the reaction completed within 2h at 50°C and afforded up to 97% isolated yield of CL as a crystalline solid. The reaction was also successfully carried out under mechanical grinding and scaled up to 20 g. The purity of the product was confirmed by melting point, FTIR, 1H-NMR and 13C-NMR spectroscopy. © 2019 Elsevier Ltd. All rights reserved. Selection and peer-review under responsibility of the scientific committee of the International Conference on Advanced Materials, Energy & Environmental Sustainability, ICAMEES2018Item Recent Advances in the Value Addition of Biomass-Derived Levulinic Acid: A Review Focusing on its Chemical Reactivity Patterns(John Wiley and Sons Inc, 2021) Dutta, S.; Bhat, N.S.Levulinic acid (LA) is one of the most prominent biomass-derived chemical building blocks that can be transformed into specialty chemicals like fuels, solvents, monomers for polymers, plasticizers, surfactants, agrochemicals, and pharmaceuticals. Over the past three decades, an enormous amount of research data have been acquired on the preparation and downstream value addition of LA, and these works have been reviewed. However, considering the astonishing number of publications appearing every year on LA derivatives, the periodical review of recent works focusing on unique aspects of chemistry must be undertaken to critically evaluate the achievements to date, reassess the challenges, and recognize new opportunities. This review discusses the chemical-catalytic synthesis of various derivatives of LA by focusing on its functionalities and reactivity patterns. Recent literature on some crucial derivatives such as γ-valerolactone, 4,4’-diphenolic acid, and ethyl levulinate have been tabulated and discussed. The synthetic interconversion between various derivatives, mechanistic insights, critical analysis of the reaction parameters toward selective preparation of various derivatives, and their potential commercial applications have been elaborated using predominantly heterogeneous catalysts. A critical assessment of the relative advantages and shortcomings of the existing synthetic strategies for various derivatives of LA has been presented to enkindle fresh ideas. © 2021 Wiley-VCH GmbHItem Hydrochloric acid-catalyzed coproduction of furfural and 5-(chloromethyl)furfural assisted by a phase transfer catalyst(Elsevier Ltd, 2020) Bhat, N.S.; Vinod, N.; Onkarappa, S.B.; Dutta, S.Furfural has been produced in 53% isolated yield from D-xylose within an aqueous HCl-1,2-dichloroethane biphasic reaction mixture using benzyltributylammonium chloride (BTBAC) as a phase transfer catalyst. The use of BTBAC noticeably improved the yield of furfural compared to that in the control reaction. The reaction was optimized on the reaction temperature, duration, concentration of HCl, and the loading of BTBAC. Furfural and 5-(chloromethyl)furfural (CMF) have also been coproduced from a mixture of pentose and hexose sugars. Under optimized conditions (100 °C, 3 h, 20.2% HCl, 10 wt% BTBAC), CMF and furfural were isolated in 17% and 53% yield, respectively, from a mixture of glucose and xylose. In addition, levulinic acid was isolated from the aqueous layer in 31% yield. © 2020 Elsevier LtdItem [Et3NH][HSO4] as an efficient and inexpensive ionic liquid catalyst for the scalable preparation of biorenewable chemicals(Springer Science and Business Media Deutschland GmbH, 2022) Bhat, N.S.; Mal, S.S.; Dutta, S.Triethylammonium hydrogen sulfate (TEAHS) has been employed as an inexpensive protic ionic liquid catalyst for the preparation of various biomass-derived renewable compounds. TEAHS efficiently catalyzed the esterification of biomass-derived chemical intermediates such as levulinic acid, 2-furoic acid, stearic acid, and isosorbide. The scalable, cosolvent-free preparations were conducted in a batch-type glass pressure reactor, which provided excellent yields (> 80%) of the esters under moderate conditions. The TEAHS catalyst was conveniently separated from the reaction mixture and reused without significant loss of activity. Graphical abstract: [Figure not available: see fulltext.] © 2020, Springer-Verlag GmbH Germany, part of Springer Nature.Item One-pot production of 5-(chloromethyl)furfural and levulinic acid from marine carbohydrates(Springer Science and Business Media Deutschland GmbH, 2025) C, P.N.; Yadav, A.K.; Aranha, D.A.; Dutta, S.5-(Chloromethyl)furfural (CMF) and levulinic acid (LA) were produced from marine biomass-derived carrageenan (? and ?) and chitin. CMF was produced in HCl (aq., 35%)-1,2-dichloroethane biphasic reaction within a batch-type glass pressure reactor, whereas LA was produced in the same setup using aqueous HCl (20%) only. The reactions were optimized on temperature, duration, stirring speed, volume of solvent, and feedstock loading. The isolated yield of CMF reached 37.8% starting from ?-carrageenan (80 °C, 2 h), whereas chitin afforded a 21.8% yield of CMF (100 °C, 4 h). LA was obtained in a 52.3% yield from ?-carrageenan (120 °C, 4 h) and 36% from chitin (150 °C, 4 h). The mixture of CMF and LA was then converted into HMF-levulinate, a prospective fuel oxygenate, in a one-pot process, affording a 77.8% isolated yield. © The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2025.Item Comprehensive utilization of crustacean wastes by chemical-catalytic transformations using levulinic acid as a sustainable platform chemical(Springer Science and Business Media Deutschland GmbH, 2025) C, P.N.; Nowl, M.S.; Mandal, S.; Dutta, S.Shell residues from seafood processing and aquaculture industries encounter significant challenges in waste management. There are many traditional and emerging applications of shell waste, but their enormous scale of production outpaces the utilization. This work reports the comprehensive utilization of shell waste by sequentially converting their major components into value-added products by selective chemical transformations. The pigments were extracted using ?-valerolactone (GVL), a biorenewable solvent produced from carbohydrate-derived levulinic acid (LA). The protein component was separated from shells under hydrothermal conditions with or without using any inorganic base. The calcite component was then reacted with LA and formic acid to form calcium levulinate and calcium formate, promising dietary supplements and chemical feedstock. Finally, chitin was converted into LA (30 mol%) under optimized conditions (150 °C, 4 h). Separation and value-addition of the components of crustacean exoskeletons demonstrated in this work are scalable, the products are marketable, and the catalyst used is recyclable. LA produced from chitin is used as the reagent and for synthesizing GVL for a closed-loop biorefinery. © The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2025.