Restrictions for pollutant emissions are getting more stringent these days due to rising environmental concerns over the world. Immense utilization of fossil fuel over past hundred years is mainly blamed as a major source of pollutants. However, despite world-wide efforts to develop alternative energy sources, fossil fuels are still considered as a major energy source. Moreover, coal consumption in the near future is expected to increase due to rapid industrialization of developing countries. In order to migrate smoothly to new energy sources with long-term visions, development of environmentally sound process to utilize fossil fuel is essential. As such efforts, removal of mineral matters and modification of coal has recently been attempted and reported. Ultra Clean Coal (UCC) project in Australia and Hyper-Coal (HPC) project in Japan recently have been demonstrated as efficient demineralization processes of coal by alkali solution treatment and organic solvent extraction respectively. Successful development of these processes would enable the direct combustion of cleaned coal powder in gas turbine of power plants which will result in both reduction of CO2 by 20% and increase of efficiency up to 48% (HHV). However, both the UCC and HPC also have obstacles for practical operation. The treated coal in the UCC process still contains 0.1 to 0.5% of ash and 60 ppm (dry coal basis) of sodium. The remained ash and sodium may cause scaling-up of ash and corrosion on turbine blades. In the HPC case, ash content in the treated coal by thermal extraction (at 360oC and 1 MPa) with organic solvent is less than 200 ppm (dry coal basis). However, a subsequent process is still needed to reduce alkali metal (Na, and K) contents to less than 0.5 ppm, which is the current acceptable level for introduction to gas turbine. Therefore, development of a feasible ion exchange process would expedite realization of the HPC process. In this study, removal of alkali metals using ion exchangers was attempted. In order to maximize overall efficiency of the HPC process, ion exchange must occur in the same condition of thermal solvent extraction (360oC, and 1 MPa). In addition, organic solvents, such as 1-MN (1-methynaphthalene) and LCO (light cycle oil), are supposed to be ion exchange mediums. Therefore, inorganic ion exchangers, which can endure such rough conditions, were prepared in our laboratory and tested. H-Y zeolite showed excellent ion exchange ability for sodium in 1-MN. However, regeneration of the used zeolite to H-Y form was complicated and expensive for a practical application. Titanium and Zirconium-based ion exchangers were also prepared with various routes. Prepared ion exchangers were first tested at room temperature in water containing sodium ions. Then, the test medium was replaced to various organic solvents at elevated temperature and pressure. This environment was provided by a custom-designed autoclave equipped with an agitator. Ion exchange capacity of each material was measured using a titration method in case of the water medium. In the organic solvent medium, remained sodium concentration in the solvent was measured by an atomic absorption spectrophotometer (AAS) and the measured concentration was converted to ion exchange capacity of the ion exchanger.