Different from other options which usually required strict conditions, a method combining atmospheric oxidization and chemical cleaning with alkali solutions was employed to desulphur coals at temperature around 90 °C. The data show that 66% organic sulphur, 44% sulphide sulphur, and 15% pyrite sulphur were lost when the coal was treated in 0.25 M NaOH at 90 °C, while the solution being aerated at the flow rate of 0.136 m 3 h −1. The rate increased to 73% for organic sulphur, 83% for sulphide sulphur and 84% for pyrite sulphur when the previous coal was further treated in acidic solution containing HCl at pH 1 for another hour. The mechanism of desulphurization was explored using inductively coupled plasma mass spectrometry, X-ray photoelectron spectroscopy and infrared. It was found out that the bond of –C S was broken by atmospheric oxygen in basic environment, leading to the lost of organic sulphur in coal. Scanning electron microscope data show that the physical structure of the coal was not adversely affected by the treatment and thermogravimetric analysis results prove that the pyrolysis behavior remained unchanged, indicating that the burning process of the coal would not be adversely affected. Unlike other oxidizing methods, this technique does not lower the heating value of the coal which was manifested by relevant data.