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Preparation of highly functionalized carbon nanoparticles using a one-step acid dehydration of glycerol

Estes, Christopher S., Gerard, Angela Y., Godward, J. Dennis, Hayes, Spencer B., Liles, Sabrina H., Shelton, Jacob L., Stewart, Tyreek S., Webster, Rebekah I., Webster, H. Francis
Carbon 2019 v.142 pp. 547-557
Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, cadmium, carbon quantum dots, catalysts, esterification, fluorescence emission spectroscopy, freeze drying, glycerol, graphene, hydrodynamics, lead, light scattering, methylene blue, moieties, oleic acid, physicochemical properties, solvents, sonication, sulfonic acid, temperature, thermogravimetry, titration, transmission electron microscopy, ultraviolet-visible spectroscopy, water pollution, water purification
In this paper, we report the low-cost synthesis of a highly functionalized carbon material synthesized through controlled acid dehydration of glycerol. Physical properties were investigated using scanning and transmission electron microscopy, X-ray diffraction, thermogravimetric analysis, and dynamic light scattering. Chemical properties were determined using elemental analysis, acid-base titration, uv–vis spectroscopy, fluorescence spectroscopy, Raman spectroscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The acid dehydration temperature during synthesis was varied and at moderate temperatures (160 °C), highly functionalized fluorescent carbon nanoparticles (hydrodynamic radius < 100 nm) containing sulfonic acid (2.6 mmol/g), carboxylic acid (2.5 mmol/g), and hydroxyl (5.8 mmol/g) functional groups were produced. Freeze-dried material prepared at this temperature could be easily dispersed in a wide range of polar solvents with sonication. The potential application as a catalyst was demonstrated and the carbon showed enhanced ability to catalyze oleic acid esterification compared to commercial catalysts. The synthesized carbon also demonstrated considerable capacity, rivaling current graphene oxide-based materials, to remove methylene blue, cadmium, and lead from contaminated water, demonstrating its potential as a nano-adsorbent for water purification. Overall, the process shown here provides a simple method to produce large quantities of a functionalized carbon nanomaterial having many potential applications.