Triboelectrostatic separation is a physical separation technique that is based on surface electronic property differences among minerals to achieve a separation. Minerals have different surface conductivities and electron affinities. They are charged differently in quantity and/or polarity after a tribocharging process. Particles with different surface charges move discretely under external electric field produce a separation. Electrostatic separation is a dry mineral processing method that does not require any water or chemical reagents. It can greatly simplify the processing circuit and reduce operating cost. Additionally, problems caused by water in conventional wet mineral processing such as water freezing, dewatering, water pollution and water treatment are eliminated. Electrostatic separation has great potential as a fine particle separator (i.e. < 1mm) in industrial minerals processing application, especially in arid areas where water supply is limited. In the current study, particle tribocharging kinetics was evaluated using a model system comprised of copper, pure coal, silica and ceramic. The results of the tribocharging process were recorded and analyzed using an oscilloscope and a signal processing technique. Charge exchange, charge separation and charge relaxation corresponding to tribocharging processes were studied using the generated pulsing signals. The signals provided a method to quantify the charge penetration into the conductor bulk during tribocharging. A new method to measure the particle surface charge using the pulsing was proposed and assessed, which was extremely useful for subtle surface charge measurements which effectively eliminated environmental noise. The interactive forces at the contacting interface, relative displacement, material electronic properties and ambient relative humidity were found to impact particle surface charge. The silica surface sites are 69 times more chargeable than the coal surface, which provides a fundamental explanation for upgrading that is achievable for silica-rich coal using triboelectrostatic separation. The influences of operating and environmental parameters were quantified and compared using an environment controlled chamber. Energy consumption at the interface was found to be positively correlated with the particle charge. Relative humidity has dual effects on the particle tribocharging, excessively low or high humidity levels do not favor particle tribocharging. Finally, a semi-empirical mathematical model of particle tribocharging was developed from the basic tribocharging compression model utilizing the parametric experiment study results. The model provides a more accurate method to predict particle surface charge under exact tribocharging conditions. A novel rotary triboelectrostatic separator (RTS) using the tribocharging mechanism was tested for upgrading fine coal. The particle size influencing the RTS tribocharging and separation process is investigated. A practical method to quantify the particle charging distribution was developed based on the direct particle charge measurement and a Gaussian distribution assumption. The smaller particles were found to have a higher average surface charge and wider surface charge distribution, which provided an opportunity to separate the high grade and the low grade coal particles. However, particles that are too small have weak particle-charger tribocharging effect that reduces particle tribocharging efficiency. The particle separation process was analyzed considering the exact experimental hydrodynamic separating conditions. Smaller particles were found to be more sensitive to the airflow that used to transport the particles as a result of the effect on residence time in the separation chamber. A method combining mathematical and statistical analysis was proposed to theoretically predict RTS separation efficiency based on the particle charging conditions and particle separation conditions. The particle horizontal displacement probability distribution was ultimately derived from this method. The model predictions indicate that a wider horizontal displacement distribution provides improved separation efficiency for the RTS unit. The theoretical analysis indicates that a particle size range between 0.105 and 0.21 mm has widest horizontal displacement distribution and thus represents an optimum particle size range which is in agreement with experimental results. The influences of the RTS operating parameters on separation performance achieved on a pure coal-silica mixture were investigated using a parametric study. The optimum operating conditions were identified. Using the optimum conditions, a five-stage separation process was conducted using the RTS unit to obtain the necessary data for the development of an ideal performance curve. Two stages of RTS separation were found to generate good quality clean coal with acceptable recovery. Particle tribocharging tests were performed using pure coal, pure silica and the coal-silica mixture as model feed materials. The test result found that mixing the pure coal with the sand reduced the particle charge distribution of the coal while increasing the charge distribution of the pure silica particle. The finding explains the inability to produce clean coal products containing ultra-low ash contents. However, the rejection of silica to the tailings stream is very high. The RTS upgrading of low-ash coal sample was tried using experiment design method, which revealed that feed rate was the most significant while the applied charger voltage and the injection air rate were the least significant in regards to product quality. Feed mass flow rate and the co-flow air rate have a significant interactive effect. Considering the theoretical findings, the impact of high feed rates is due to the negative effect on particle tribocharging efficiency resulting from an increase in the particle-particle surface charge relaxation. Under the optimum test conditions, an ultraclean coal was produced with an ash content of 3.85±0.08% with a combustible recovery of 62.97±1.11% using the RTS unit.