A novel flame retardant
(TDA) containing phosphorus, nitrogen,
and silicon was synthesized successfully via a controllable ring-opening
addition reaction between 1,3,5-triglycidyl isocyanurate, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide,
and 3-aminopropyltriethoxysilane, and TDA was then blended with diglycidyl
ether of bisphenol A to prepare flame-retardant epoxy resins (EPs).
The chemical structure and components of TDA were confirmed by Fourier
transform infrared (FTIR) spectra,
31
P nuclear magnetic
resonance, and X-ray photoelectron spectroscopy. Thermogravimetric
analysis results indicated that after the introduction of TDA, cured
EP maintained good thermal stability with a minimum initial decomposition
temperature of 337.6 °C, and the char yields of a EP/TDA-5 sample
significantly increased by 76.2% compared with that of the neat EP
thermoset. Additionally, with the addition of 25.0 wt % TDA (1.05
wt % phosphorus loading), the limited oxygen index value of cured
EP increased from 22.5% of pure EP to 33.4%, and vertical burning
V-0 rating was easily achieved. Meanwhile, after the incorporation
of TDA, the total heat release and total smoke production of the EP/TDA-5
sample obviously reduced by 28.9 and 27.7% in the cone calorimeter
test, respectively. Flame-retardant performances and flame-retardant
mechanisms were further analyzed by scanning electron microscopy,
FTIR, energy-dispersive spectrometry, and pyrolysis gas chromatography/mass
spectrometry. The results reveal that the synergistic effect of phosphorus,
nitrogen, and silicon plays an excellent flame-retardant role in both
gaseous and condensed phases. In addition, the mechanical and dynamic
mechanical properties of cured EP thermosets are well maintained rather
than destroyed. All the results demonstrate that TDA endows epoxy
resin with excellent flame retardancy and possesses great promise
in the industrial field.