A Study on Exfoliation of Expanded Graphite Stacks in Candelilla Wax

A novel, green route for pre-exfoliation of graphite based on a biodegradable polymer and high-power ultrasound is presented. Candelilla wax (CW), derived from the leaves of the candelilla plant, has been used for the first time as a natural non aqueous medium to induce the pre-exfoliation of expanded graphite (EG) under ultrasonic irradiation in an economical way. The proposed method uses also D-limonene as a natural organic solvent for reducing viscosity and increasing the affinity between the polar groups of EG and candelilla wax, thus improving the intercalation/exfoliation of EG. The quality of dispersion of the nanofiller in the natural wax matrix has been evaluated using multiple techniques. The addition of EG to wax and use of ultrasonic treatment leads to a reduced crystallinity, probably due to restrictions of the molecular movements, improved thermal stability of wax, and to an increased shear thinning exponent, which are all indicative of a high degree of EG dispersion. The ultrasonic dynamic mechanical results suggest a reduction in the cluster size and a better filler dispersion in the wax matrix promoted by polar or chemical reactions between the CW fractions and the graphite stacks, which was observed by XPS analysis. The results were compared to those obtained with paraffin, a synthetic wax, and confirmed the dispersion improvement obtained by using natural wax as a pre-exfoliating medium.