Flame-retardant behavior and mechanism of a DOPO-based phosphorus–nitrogen flame retardant in epoxy resin

Abstract

A novel flame-retardant additive, 6,6′,6″-((1,3,5-triazine-2,4,6 triyl) tris (azanediyl)) tris (dibenzo[c,e][1,2]oxaphosphinine 6-oxide) (DOPO-M), was synthesized from melamine and 9,10-dihy-dro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO). The structure of DOPO-M was characterized by Fourier transform infrared (FTIR) spectroscopy, proton (1H) and phosphorous (31P) nuclear magnetic resonance (NMR) spectroscopies, and electrospray ionization mass spectroscopy (ESI-MS). DOPO-M was blended into epoxy resin (EP) to prepare flame-retardant EPs. The flame-retardant and thermal properties of EPs cured with triethylenetetramine (TETA) were investigated by thermogravimetric analysis (TGA), the UL-94 test, and the limiting oxygen index (LOI) test. The results revealed that the epoxy thermosets exhibited excellent flame retardancy and passed the V-0 rating of the UL-94 test with an LOI of 29.3% when the phosphorus content was 2.57 wt%. The scanning electron microscopy (SEM) results showed that DOPO-M in the EP/TETA system obviously accelerated the formation of a stronger, phosphorus-rich sealing char layer to improve the flame-retardant properties of the matrix during combustion.