Phosphate tailings (PTs) are solid waste, which is produced by phosphate flotation. In this work, PTs were used as raw materials for the preparation of diethylenetriamine pentamethronic acid (DTPMP) intercalated trimetal (Ca-Mg-Al) layered double hydroxides (TM-DTPMP LDHs) by co-precipitation method. TM-DTPMP LDHs were characterized by X-ray diffraction, fourier-transform infrared spectroscopy, scanning electron microscopy, differential thermal gravimetric analysis, X-ray photoelectron spectroscopy and applied as a flame retardant to improve the fire safety of epoxy resin (EP). The results showed that the composite materials exhibited obvious layered structure. After intercalation, layer spacing increased from 0.783 to 1.78 Å. When the amount of TM-DTPMP LDH in EP was 8%, the limitted oxygen index of the composite material increased from the original 19.2% to 30.2%. In addition, Cone calorimeter (CC) and Raman spectrum results indicated that with the addition of TM-DTPMP LDHs, the value of heat release rate peak (pHRR) and total heat release (THR) were reduced by more than 43% and 60%, while the value of smoke formation rate (pSPR) and the total smoke production (TSP) decreased nearly 64% and 83%, respectively. The significant reduction in the release of combustion heat and harmful smoke during EP combustion may be attributed to the synergistic flame-retardant effect between hydrotalcite and DTPMP. This work exhibited great potential for the green recycling of PTs and the enhancement of the fire safety of EP.
In this work, phosphate tailings (PTs) were used as raw materials for the preparation of Ca-Mg-Al layered double hydroxides (LDHs-1) and Ca-Mg-Al-Fe layered double hydroxides (LDHs-2) by co-precipitation method. The as-prepared samples were characterized by FT-IR, SEM, XRD, and XPS and applied as a flame retardant to improve the fire safety of epoxy resin (EP). The results showed that both LDHs-1 and LDHs-2 exhibited layered structure and high crystallinity. Compared with neat EP, the value of limiting oxygen index (LOI) increased from 25.8 to 29.3 and 29.9 with 8 wt% content of LDHs-1 and LDHs-2, respectively. The flame retardant properties of the composite material were characterized by cone calorimeter (CC), and the results showed that the peak value of the smoke production rate (SPR) decreased more than 45% and 74%, total smoke production (TSP) reduced nearly 64% and 85% with the addition of LDHs-1 and LDHs-2. Meanwhile, the value of the total heat release (THR) reduced more than 28% and 63%. The conversion from LDHs to layered double oxide (LDO) might be conducive to the fire safety of EP. Moreover, the transformation of Fe-OH to Fe-O could promote the early cross-linking of polymer. In summary, LDHs-2 could significantly improve the carbonization process of EP and suppress the smoke released during the combustion process.
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