Developing superior properties of epoxy resin composites with high fire resistance, light smoke, and low toxicity has been the focus of the research in the flame-retardant field. In particular, it is essential to decrease the emissions of toxic gases and smoke particles generated during the thermal decomposition of epoxy resin (EP) to satisfy the industrial requirements for environmental protection and safety. Consequently, the PZS@ZIF-67 composite was designed and synthesized by employing the hydroxyl group-containing polyphosphazene (poly(cyclotriphosphazene-co-4,4′-dihydroxydiphenylsulfone), PZS) as both the interfacial compatibility and an in situ template and the ZIF-67 nanocrystal as a nanoscale coating and flame-retardant cooperative. ZIF-67 nanocrystal with multidimensional nanostructures was uniformly wrapped on the surface of PZS microspheres. Subsequently, the acquired PZS@ZIF-67 composite was incorporated into the epoxy resin to prepare composite samples for the study of their fire safety, toxicity suppression, and mechanical performance. Herein, the EP/5% PZS@ZIF-67 passed the V-0 rating in a UL-94 test with a 31.9% limit oxygen index value. More precisely, it is endowed with a decline of 51.08%, 28.26%, and 37.87% of the peak heat release rate, the total heat release, and the total smoke production, respectively. In addition, the unique structure of PZS@ZIF-67 microsphere presented a slight impact on the mechanical properties of EP composites at low loading. The PZS@ZIF-67 possible flame-retardant mechanism was speculated based on the analysis of the condensed phase and the gas phase of EP composites.
A new strategy for the preparation of an integrated three-source intumescent flame retardant (IFR) has been developed to improve the flame-retardant and smoke suppression performance of epoxy resin (EP) with a synergistic flame retardant effect. Herein, the synthesis of a macromolecular spirocyclic phosphorus/nitrogen-containing IFR poly sulfonamide spirocyclic pentaerythritol bisphosphonate (SAPC) is reported via a two-step method that uses pentaerythritol, phosphorus oxychloride and sulfonamide (SAA) as raw materials. Subsequently, the SAPC was incorporated into EP to prepare the composite to investigate its thermal stability, flame retardancy, and smoke suppression performance. Herein, a differential scanning calorimetry (DSC) analysis showed that the addition of SAPC increased the glass transition temperature (Tg) of the composite. Cone test results indicated that the incorporation of 8 wt % SAPC significantly improved the flame-retardant performance for the composite, with a 43.45% decrease in peak of heat release rate, a 28.55% reduction in total heat release, and a 30.04% decrease in total smoke release. Additionally, the composite received the V-0 rating in a UL-94 vertical burning test, accompanied by the “blowout” phenomenon. After the addition of SAPC, the amount of flammable gas products from the EP composite decomposition was obviously suppressed, and the amount of non-flammable as was increased. All of this suggests a good dilution role of SAPC. There are enough reasons to believe that the enhanced flame-retardant and toxicity suppression performance for the EP composite can be attributed to the good coordination of carbonization agent, acid source, and blowing agent in the SAPC structure.
Derivatives of 3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro-[5,5]undecane-3,9-dioxide (SPDPC) are of increasing interest as flame retardants for polymeric materials. In addition, SPDPC is also an important intermediate for the preparation of intumescent flame retardants (IFRs). However, low efficiency and undesirable dispersion are two major problems that seriously restrain the application of IFRs as appropriate flame retardants for polymer materials. Usually, the functionalization or modification of SPDPC is crucial to acquiring high-performance polymer composites. Here, a small molecule spirocyclic flame retardant diphenylimidazole spirocyclic pentaerythritol bisphosphonate (PIPC) was successfully prepared through the substitution reaction between previously synthesized intermediate SPDPC and 2-phenylimidazole (PIM). Phenyl group and imidazole group were uniformly anchored on the molecular structure of SPDPC. This kind of more uniform distribution of flame retardant groups within the epoxy matrix resulted in a synergistic flame retardant effect and enhanced the strength of char layers to the epoxy composites, when compared to the unmodified epoxy. The sample reached a limiting oxygen index (LOI) of 29.7% and passed with a V-0 rating in the UL 94 test with the incorporation of only 5 wt % of as-prepared flame retardant PIPC. Moreover, its peak of heat release rate (pHRR) and total heat release (THR) decreased by 41.15% and 21.64% in a cone calorimeter test, respectively. Furthermore, the addition of PIPC has only slightly impacted the mechanical properties of epoxy composites with a low loading.
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