Synthesis of hexakis (γ-aminopropylsilanetriol) cyclotriphosphazene and application in intumescent flame retardant polypropylene
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Abstract
A novel charring agent named as hexakis (γ-aminopropylsilanetriol) cyclotriphosphazene (HKHPCP) was synthesized by using hexachlorocyclotriphosphazene (HCCP), p-hydroxy benzaldehyde and γ-aminopropylsilanetriol (KH553). The intumescent flame retardant polypropylene (PP) matrix composites (APP-HKHPCP-NOR116/PP) was prepared using HKHPCP and ammonium polyphosphate (APP) as the anti-dripping agent and N-alkoxy hindered amine (NOR116) as the synergistic agent by the melt compounding method. The chemical structures of intermediate and HKHPCP were characterized by FTIR, 1H nuclear magnetic resonance (1H NMR) and 31P NMR. The effects of the flame retardant APP-HKHPCP-NOR116/PP on the thermal degradation, flame retardancy and char layer structure were investigated by thermogravimetric analysis (TGA), limiting oxygen index (LOI), vertical burning test (UL-94), cone calorimetric test, SEM and laser Raman spectroscopy, respectively. The TGA results show that the temperature of 5% mass loss of HKHPCP in oxygen is 300.2℃, and the residues at 1 000℃ of HKHPCP in oxygen is 34.8%. The results show that the LOI value of APP-HKHPCP-NOR116/PP is 43%, while the intumescent flame retardant loading is 30wt%. The APP-HKHPCP-NOR116/PP could reach a V-0 rating in the UL-94 tests. The cone calorimetry results indicate that heat release rate (HRR), total heat release (THR), smoke produce rate (SPR) and total smoke production (TSP) are reduced by 75.0%, 50.5%, 88.0% and 80.8%, respectively. In addition, the APP-HKHPCP-NOR116/PP can form a compact and more graphitic carbon char layer during combustion.
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