Solid ash-free coal (AFC) samples recovered from solvent-extracted solution by vacuum drying, dilution precipitation and spray drying methods were compared in terms of physical properties and chemical structure. AFC was prepared by using Kideco coal (Indonesian sub-bituminous coal) and polar N-methyl-2-pyrrolidone (NMP) solvent as raw materials. The physical properties of the AFCs were characterized with proximate, ultimate, and calorific value analysis. In analyzing the chemical structure, FTIR and NMR were used. the proximate analysis showed much reduced ash in the AFCs compared to parent raw coal. The FTIR result showed that the extraction solvent was not fully removed from the AFC prepared by vacuum drying. However, the solvent was not detected in the AFC recovered by using dilution precipitation. Dilution precipitation has advantages over the other two methods, since it can be done at relatively low temperature and separate ash-free coal from extraction solvent more effectively.