Abstract: In response to the complex composition, high ash and carbon contents, and clean utilization barriers of coal liquefaction residues, petroleum ether, methanol, cyclohexane, carbon disulfide (CS₂), benzene, and isometric acetone/CS₂ were used to extract soluble organics from Xinjiang Heishan coal liquefaction residue by the ultrasonic-assisted extraction at mild condition, based on the exceptional solubility of coal liquefaction residue in organic solvents. FTIR spectroscopy coupled with GC/MS analysis was applied to reveal the compositional and structural characteristics of the soluble organics from coal liquefaction residue. The result shows that fractional extraction can sequentially weaken the different intermolecular forces of organic compounds in coal liquefaction residue, achieving the separation of group components of organic compounds in coal liquefaction residue with the total yield of 60.9%. The highest yield is 24.9% from CS₂. The soluble organic matter is typically characterized by condensed aromatic ring structures containing 4-6 benzene rings. The oxygen-containing compounds exhibit considerable diversity, primarily comprising functional groups such as phenolic hydroxyl, alcoholic hydroxyl, alkoxy, ether bridges, ester groups, and ketone carbonyl groups. Sulfur predominantly exists in the form of thiophene rings, while long-chain alkanes are entrapped or encapsulated within the macromolecular network structure.