To endow synergistically epoxy resin (EP) with excellent fire resistance and high optical transparency, a nitrogen-rich DOPO-based derivate (named as FATP) was synthesized and incorporated into EP. It showed that the incorporation of the FATP reduced the fire hazard of the EP, as demonstrated by the fact that the EP/4% FATP blends gained a UL-94 V-0 rating and an LOI value of 35%, with the lowest values of the THR (86.7 MJ/m2), the PHRR (1059.3 kW/m2), and the TSP (89.6 MJ/m2). The presence of the FATP also reduced the thermal stability and the crosslinking density whilst improving the curing reaction and the storage modulus of the EP/FATP blends. The TG-FTIR spectra showed that •HPO/•PO free radicals and some nonflammable gases (HN3 and NH3) were produced during the pyrolysis, and the characterization (SEM, Raman spectroscopy, and XPS) of char residues confirmed that the FATP facilitated the formation of continuous and compact carbon layers of greater graphitization degree. It was thus concluded that the FATP played the flame-retardant roles in both the gas and condensed phases. Furthermore, the FREPs kept almost identical transparency as the pristine EP, and mechanical properties were also slightly enhanced. The FREPs presented in this work show promising applications in the fields of advanced optical technology.
A compound containing phosphorus/nitrogen/sulfur (named as DOVNPT) was synthesized by the reaction of p-toluenesulfonamide, vanillin and 9,10-dihydro-9-oxo-10-phosphophenanthrene-10-oxide, and was adopted to prepare flame retardant epoxy resins (FREPs) using 4,4-diaminodiphenylmethane as the curing agent. The chemical structure of DOVNPT was verified using Fourier-transform infrared spectroscopy, 1 H and 31 P nuclear magnetic resonance. The influence of the DOVNPT content on the thermal stability, fire performance, combustion behaviors, transparency and mechanical properties of the FREPs was investigated in detail. The DOVNPT promoted the decomposition of EP on advance whilst lowered the maximum decomposition rate. With the incorporation of 4 wt% DOVNPT (0.49 wt% phosphorus content), the FREP-4 achieved a LOI value of 34.4% and a UL-94 V-0 rating. The FREP-4 also gave the lowest peak heat release rate, total heat release and total smoke release, with a reduction of 40.4%, 24.8%, and 28.6% as compared with the pure EP, respectively. The comprehensive analysis of the char residues and gaseous pyrolysis products demonstrated that the DOVPNT displayed good flame retardant effect in both gas phase and condensed phase. Simultaneously, the FREPs presented a comparable transparency and slightly improved mechanical properties as compared with the pure EP.
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