The present study aimed to understand the pyrolysis characteristics of phosphorus tailings and promote the resource utilization of phosphorus tailings. Thermogravimetry was combined with Fourier transform infrared spectroscopy-Raman spectroscopy-mass spectrometry (TG-FTIR-RS-MS) and kinetic models to investigate the possible reaction mechanisms during the pyrolysis of phosphorus tailings and the changes in the release characteristics of pyrolysis volatiles. The results showed that the pyrolysis process occurred in three different stages. First, small amounts of adsorbed water were removed, and organic matter in the tailings was decomposed. Second, CaMg(CO3)2 underwent thermal decomposition to produce CaCO3, MgO, and CO2. Third, CaCO3 further decomposed into CaO and CO2. Similarly, the pyrolysis kinetics were divided into three intervals based on the differences in their activation energy values. The pyrolysis reaction mechanism functions were two-dimensional diffusion (Valensi model), nucleation and growth (Avrami-Erofeev, n = 1/2), and nucleation and growth (Avrami-Erofeev, n = 1/4). The gases released during the pyrolysis of phosphate tailings were mainly CO2, F2, and HF.
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