In this paper, phosphated K-carrageenan (P-KC) was obtained by reacting POCl3 with the renewable source K-carrageenan (KC). P-KC and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) were added into waterborne epoxy (EP) to improve its flame retardancy. The structure of P-KC was studied comprehensively using Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), thermo-gravimetric analysis (TGA), showing the successful synthesis of P-KC. The flame retardancy of the EP was evaluated by the cone calorimeter test. The results showed that different mass ratios of DOPO and P-KC affected the flame retardancy of EP. When the mass ratio of DOPO and P-KC was 2:1, total heat release (THR) and total smoke production (TSP) decreased by 48.7% and 37.4%, respectively. The microstructures of residue char were observed by FTIR and scanning electron microscopy (SEM), indicating that the flame-retardant waterborne epoxy (FR-EP) system held a more cohesive and denser char structure. The char inhibited the diffusion of heat and oxygen, which played a key role in the flame retardancy.
In this article, the intumescent flame-retardant microsphere (KC-IFR) was prepared by inverse emulsion polymerizations, with the use of k-carrageenan (KC) as carbon source, ammonium polyphosphate (APP) as acid source, and melamine (MEL) as gas source. Meanwhile, benzoic acid functionalized graphene (BFG) was synthetized as a synergist. A “four-source flame-retardant system” (KC-IFR/BFG) was constructed with KC-IFR and BFG. KC-IFR/BFG was blended with waterborne epoxy resin (EP) to prepare flame-retardant coatings. The effects of different ratios of KC-IFR and BFG on the flame-retardant properties of EP were investigated. The results showed that the limiting oxygen index (LOI) values increased from 19.7% for the waterborne epoxy resin to 28.7% for the EP1 with 20 wt% KC-IFR. The addition of BFG further improved the LOI values of the composites. The LOI value reached 29.8% for the EP5 sample with 18 wt% KC-IFR and 2 wt% BFG and meanwhile, UL-94 test reached the V-0 level. In addition, the peak heat release (pHRR) and smoke release rate (SPR) of EP5 decreased by 63.5% and 65.4% comparing with EP0, respectively. This indicated the good flame-retardant and smoke suppression property of EP composites coating.
A k-carrageenan–iron complex (KC–Fe) was synthesized by complexation between degraded KC and FeCl3. Furthermore, KC–Fe and ammonium polyphosphate (APP) were simultaneously added into waterborne epoxy (EP) to improve its flame retardancy and smoke suppression performance. The structure and properties of KC–Fe were assessed using Fourier transform infrared spectroscopy (FTIR), ultraviolet (UV) spectroscopy, thermo gravimetric analysis (TGA), and X-ray powder diffraction analysis (XRD). The analysis showed that KC–Fe was successfully synthesized and exhibited good thermal properties with a 49% char residue at 800 °C. The enhanced flame retardancy and smoke suppression performance of waterborne epoxy were evaluated using a limiting oxygen index (LOI) and UL-94. Moreover, the flame retardancy of waterborne epoxy coated on a steel plate was also investigated using cone calorimetry. The results showed that the flame-retardant waterborne epoxy blend exhibited the best flame retardancy when the mass ratio of APP and KC–Fe was 2:1. The total heat release (THR) and total smoke production (TSP) was decreased by 44% and 45%, respectively, which indicated good fire safety performance and smoke suppression properties. Analysis of the residual char using FTIR, SEM, and elemental analysis (EDS) indicated that the action of KC–Fe was promoted by the presence of APP. The formation of a dense thermal stable char layer from an intumescent coating was essential to protect the underlying materials.
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