In order to efficiently use Xinjiang changyan coal (XCC), thermal dissolution (TD) of XCC was carried out in a mixed solvent of toluene/ethanol, and the dissolved matters were further separated with medium-pressure liquid chromatography (MPLC). Seventy-three aromatics including 25 one-benzene-ring aromatics, 39 two-benzene-ring aromatics, and 9 three-benzene-ring aromatics were enriched and then analyzed with gas chromatography/mass spectrometry (GC/MS). The isolation and analysis of these high-valued aromatics could provide an important theoretical basis for non-fuel use of low-rank coals.