Synthesis and carbonization chemistry of a phosphorous–nitrogen based intumescent flame retardant

In this work, a polymeric phosphorous–nitrogen containing intumescent flame retardant, named poly(diaminodiphenyl methane spirocyclic pentaerythritol bisphosphonate) (PDSPB), was synthesized. The carbonization chemistry was investigated. FTIR and 1H NMR were used to confirm the chemical structure of PDSPB. Thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), in situ FTIR and energy dispersive X-ray (EDX) were used to investigate and monitor the chemical structural changes during thermal degradation. PDSPB demonstrated a three-step degradation behavior. PDSPB oligomers continuously polymerized and generated a higher macromolecular weight during the first step (200–250 °C). The phosphate ester bonds were broken down and phosphoric acid was released which dehydrated the carbon source to form chars during the second step (280–320 °C). The residues will be further degraded and form final chars during the final weight loss step (400–450 °C). The final chars showed a complex P—O—Ph and aromatic/graphitic structure containing architecture.