The zeolite production process is currently being very intensively researched. Due to environmental protection, as well as issues related to the guidelines of a zero-waste economy, all activities aimed at obtaining such materials from post-processed waste are extremely important. This article presents an innovative method of utilising calcined carboniferous shale in order to produce synthetic zeolites. The raw material for testing came from two Polish hard coal mines. Both the chemical and phase composition of the coal shale were characterised. Based on the recorded thermal analysis results coupled with the mass spectrometer, the processes occurring during the heating of raw materials were interpreted and the calcination temperatures were determined. The changes in the phase composition of raw materials resulting from the calcination process used were also analysed. The heat-treated raw materials were subjected to the synthesis of zeolites in an aqueous solution of sodium hydroxide by means of the hydrothermal method at a concentration of 2.75 M. The results of water leaching and structural parameters are presented for both raw materials, as well as the produced synthesis. The conducted research confirmed that after the application of the synthetic process on coal shale, a zeolite with a surface area of equal to 172 m/g can be obtained.