Synthesis and characterization of SPDSCD and its flame retardant application on epoxy resins

Abstract

In this study, a flame retardant agent, 2,4,8,10-tetraoxo-3,9-diphosphospiro[5.5]undecane spirophosphate-4,4-diaminopair benzene disulfone-1,3,5-himetriazine (SPDSCD), is synthesized through a direct polycondensation reaction. SPDSCD is a chemically expanded phosphorus-containing flame retardant in epoxy resins (EP). The molecular structure of SPDSCD and thermal stability are characterized by nuclear magnetic resonance, Fourier transform infrared spectroscopy, and thermogravimetric analysis, and EP/SPDSCD composites were investigated in detail. These properties are associated with the phosphorus-containing spiro structure on the main molecular chain which can promote condensation polymerization into carbon during pyrolysis, the new nitrogen-containing carbon source, and the triazine structure. SPDSCD shows good thermal stability and low flammability, the weight loss from 500 to 800 °C was only 6.1 wt%, and the residual mass at 800 °C was 48.9 wt%. With the addition of SPDSCD, the flame retardant quality of the composites was gradually enhanced, the carbon residue becomes denser, which isolates heat transfer and inhibits the volatilization of flue gas. The addition of 20 wt% SPDSCD in the EP sample was associated with a limited oxygen index (LOI) value of 26% and a vertical burning V-0 rating. Cone calorimeter test shows that the peak heat release rate is reduced by 75%; the heat release rate curve enters the heat release platform area with a value lower than the first peak, TSP is reduced by 24%, the ac-CO₂Y value reduced by 25.6%, indicating that SPDSCD/EP produced less CO₂, which obviously prevented the combustion of volatile gas. SPDSCD exerted a charring and barrier effect in the condensation phase. Using basic characterization and flame retardancy testing, this work determined that SPDSCD has good flame retardancy when added to EP.