4.6 Article

Synthesis and Characterization of Sulfonated Carbon-Based Graphene Oxide Monolith by Solvothermal Carbonization for Esterification and Unsymmetrical Ether Formation

Journal

ACS SUSTAINABLE CHEMISTRY & ENGINEERING
Volume 4, Issue 4, Pages 1963-1973

Publisher

AMER CHEMICAL SOC
DOI: 10.1021/acssuschemeng.5b01205

Keywords

Graphene oxide; Solvothermal synthesis; Sulfated carbon-based graphene oxide monolith; Esterification; Heterogeneous catalyst

Funding

  1. CSIR

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Herein, we report solvothermal carbonization of biomass, such as glucose, in the presence of a small amount of graphene oxide (GO) as a structure directing agent that yields a carbon-based graphene oxide monolith (CGO monolith). The CGO monolith was functionalized with chlorosulfonic acid under mild reaction conditions to achieve sulfated carbon-based graphene oxide (SO3H@ CGO monolith). It was used for the esterification of levulinic acid with benzyl alcohol and the etherification of benzyl alcohol with butanol as model reactions. The activity of the catalyst was compared with different solid acid catalysts, such as GO, CGO monolith, nanocrystalline sulfated titania (NCST), SO3H@HTC (sulfated hydrothermal carbon), amberlyst-15, and SO3H@GO for esterification of levulinic acid with benzyl alcohol. The SO3H@CGO monolith showed excellent conversion (97%) toward benzyl levulinate at 110 degrees C with low catalyst loading (0.008 g/cm(3)) and mole ratio. The catalyst was well characterized by SEM, EDXA, TEM, XRD, FTIR, BET surface area, CHNS, and TGA analysis. The role of various parameters, such as speed of agitation, molar ratio, catalyst loading, and temperature, on the reaction rate using SO3H@CGO monolith as catalyst was studied to establish the mechanism of the reaction, and the catalyst was reused up to five times, including the fresh one. The overall process is novel and green.

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