Abstract
Spent coffee grounds (SCG) valorisation can produce high-value products to supply cosmetics, petroleum and pharmaceutical industries among others. An overview of the various products achievable from spent coffee grounds valorisation are established, while the effect of temperature, reaction time and solid-to-liquid loading ratio on the yield of caffeine extracted from SCG was investigated. The best extraction solvent between (i) dichloromethane, (ii) 1-ethyl-3-methylimidazolium chloride (IL) and (iii) water was established. Characterisation of SCG using Technical Association of the Pulp and Paper (TAPPI) methods was carried out. Variations of parameters were established using the Box-Behnken design of experiment (DOE) which varied the investigated parameters; (i) temperature (88 – 120 ºC), (ii) reaction time (15 - 35 min) and (iii) solid-to-liquid loading ratio (5 g SCG per 10 -25 mL). The conventional extraction method used dichloromethane as the extraction solvent, whereas the green method used the ionic liquid and water in a Parr pressure reactor. High performance liquid chromatography (HPLC) quantified the yield of extracted caffeine. Recrystallised caffeine is analysed using scanning electron microscopy (SEM), transition electron microscopy (TEM) and energy dispersive spectroscopy (EDS) for its structural properties, crystalline structure and physical analysis, while differential scanning calorimetry (DSC) established the purity of extracted caffeine achieved from each extraction solvent. The expected yield of caffeine is between 4.67 and 8.0 mg/g SCG. According to this experimental methodology, at 120 ºC, 25 min reaction time and 25 mL solvent volume the extraction yield ranged from 2.83 to 3.67 mg/g SC
