A Rapid and Green Method for the Preparation of Solketal Carbonate from Glycerol

Glycerol is a biogenic waste that is generated in both the biodiesel and oleo-chemical industries. The value addition of surplus glycerol is of utmost importance for making these industries economically profitable. In line with this, glycerol is converted into glycerol carbonate, a potential candida...

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Main Authors: Sanjib Kumar Karmee, Sreedhar Gundekari, Louis C. Muller, Ajinkya Hable
Format: Article
Language:English
Published: MDPI AG 2025-02-01
Series:Reactions
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Online Access:https://www.mdpi.com/2624-781X/6/1/15
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author Sanjib Kumar Karmee
Sreedhar Gundekari
Louis C. Muller
Ajinkya Hable
author_facet Sanjib Kumar Karmee
Sreedhar Gundekari
Louis C. Muller
Ajinkya Hable
author_sort Sanjib Kumar Karmee
collection DOAJ
description Glycerol is a biogenic waste that is generated in both the biodiesel and oleo-chemical industries. The value addition of surplus glycerol is of utmost importance for making these industries economically profitable. In line with this, glycerol is converted into glycerol carbonate, a potential candidate for the industrial production of polymers and biobased non-isocyanate polyurethanes. In addition, glycerol can also be converted into solketal, which is the protected form of glycerol with a primary hydroxyl functional group. In this contribution, we developed a microwave-assisted solvent and catalyst-free method for converting solketal into solketal carbonate. Under conventional heating conditions, the reaction of solketal with dimethyl carbonate resulted in 70% solketal carbonate in 48 h. However, under microwave heating, 90% solketal carbonate was obtained in just 30 min. From the perspective of sustainability and green chemistry, biomass-derived heterogeneous catalysts are gaining importance. Therefore, in this project, several green catalysts, such as molecular sieves (MS, 4Å), Hβ-Zeolite, Montmorillonite K-10 clay, activated carbon from groundnut shell (<i>Arachis hypogaea</i>), biochar prepared from the pyrolysis of sawdust, and silica gel, were successfully used for the carbonyl transfer reaction. The obtained solketal carbonate was thoroughly characterized by <sup>1</sup>H NMR, <sup>13</sup>C NMR, IR, and MS. The method presented here is facile, clean, and environmentally benign, as it eliminates the use of complicated procedures, toxic solvents, and toxic catalysts.
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spelling doaj-art-ab1dc2bfdd48443a8e0e5db28f0b334c2025-08-20T03:43:57ZengMDPI AGReactions2624-781X2025-02-01611510.3390/reactions6010015A Rapid and Green Method for the Preparation of Solketal Carbonate from GlycerolSanjib Kumar Karmee0Sreedhar Gundekari1Louis C. Muller2Ajinkya Hable3The Odisha Renewable Energy Research Institute (ORERI), Subarnapur 767018, Odisha, IndiaDepartment of Engineering Chemistry, Koneru Lakshmaiah Education Foundation, KL (Deemed to be) University, R.V.S Nagar, Moinabad-Chilkur Rd, Aziznagar 500075, Telangana, IndiaSchool of Energy Resources, University of Wyoming, Laramie, WY 82071, USAThe Odisha Renewable Energy Research Institute (ORERI), Subarnapur 767018, Odisha, IndiaGlycerol is a biogenic waste that is generated in both the biodiesel and oleo-chemical industries. The value addition of surplus glycerol is of utmost importance for making these industries economically profitable. In line with this, glycerol is converted into glycerol carbonate, a potential candidate for the industrial production of polymers and biobased non-isocyanate polyurethanes. In addition, glycerol can also be converted into solketal, which is the protected form of glycerol with a primary hydroxyl functional group. In this contribution, we developed a microwave-assisted solvent and catalyst-free method for converting solketal into solketal carbonate. Under conventional heating conditions, the reaction of solketal with dimethyl carbonate resulted in 70% solketal carbonate in 48 h. However, under microwave heating, 90% solketal carbonate was obtained in just 30 min. From the perspective of sustainability and green chemistry, biomass-derived heterogeneous catalysts are gaining importance. Therefore, in this project, several green catalysts, such as molecular sieves (MS, 4Å), Hβ-Zeolite, Montmorillonite K-10 clay, activated carbon from groundnut shell (<i>Arachis hypogaea</i>), biochar prepared from the pyrolysis of sawdust, and silica gel, were successfully used for the carbonyl transfer reaction. The obtained solketal carbonate was thoroughly characterized by <sup>1</sup>H NMR, <sup>13</sup>C NMR, IR, and MS. The method presented here is facile, clean, and environmentally benign, as it eliminates the use of complicated procedures, toxic solvents, and toxic catalysts.https://www.mdpi.com/2624-781X/6/1/15biodieselglycerolsolketalmicrowavesolketal carbonategreen chemistry
spellingShingle Sanjib Kumar Karmee
Sreedhar Gundekari
Louis C. Muller
Ajinkya Hable
A Rapid and Green Method for the Preparation of Solketal Carbonate from Glycerol
Reactions
biodiesel
glycerol
solketal
microwave
solketal carbonate
green chemistry
title A Rapid and Green Method for the Preparation of Solketal Carbonate from Glycerol
title_full A Rapid and Green Method for the Preparation of Solketal Carbonate from Glycerol
title_fullStr A Rapid and Green Method for the Preparation of Solketal Carbonate from Glycerol
title_full_unstemmed A Rapid and Green Method for the Preparation of Solketal Carbonate from Glycerol
title_short A Rapid and Green Method for the Preparation of Solketal Carbonate from Glycerol
title_sort rapid and green method for the preparation of solketal carbonate from glycerol
topic biodiesel
glycerol
solketal
microwave
solketal carbonate
green chemistry
url https://www.mdpi.com/2624-781X/6/1/15
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