Evaluating the heat resistance of thermal insulated sandwich composites subjected to a turbulent fire

The fire structural response of sandwich composite laminates incorporating bio‐derived constituents subjected to a turbulent flaming fire was investigated. Fire structural tests were conducted on thermal insulated sandwich composites incorporating a thin surface‐bonded non‐woven glass fibre tissue impregnated with char‐forming fire retardant, ammonium polyphosphate. The sandwich composite laminates were loaded in compression at 10%, 15% or 20% of the ultimate compressive strength while simultaneously subjected to turbulent flames imposing an incident heat flux of 35 kW/m². Generally, the failure time increased with the reduced applied compressive load. The thermal insulated sandwich composite laminates had considerably improved fire resistance in comparison to their unmodified counterparts. The unmodified composites failed 96 s earlier than the thermal insulated specimens when the compression load was 10% of the ultimate compressive strength. The presence of ammonium polyphosphate at the heat‐exposed surface promoted the formation of a consolidated char layer, which slowed down heat conduction into composite laminate substrate. The fire reaction parameters measured via the cone calorimeter provided insights into the thermal response hence fire structural survivability of sandwich composite laminates. Copyright © 2015 John Wiley & Sons, Ltd.     

A simplified model for predicting the ignition of FRP composites with validation using intermediate‐scale fire experiment data

This study presents a simplified theoretical model to predict the ignition of FRP composites of general thermal thickness (GTT) subjected to one‐sided heating. A simplified GTT heat transfer model to predict the surface temperature of GTT composite panels was developed, and the exposed surface temperature was used as ignition criterion. To validate the GTT model, intermediate scale calorimeter fire tests of E‐glass fiber reinforced polyester composite panels at three heat flux levels were performed to obtain intermediate‐scale fire testing data in a controlled condition with well‐defined thermal boundary conditions. The GTT model was also verified by using results from finite element modeling predictions. This model can be used to estimate the surface temperature increase, time‐to‐ignition, and mass loss of FRP composites for fire safety design and analysis. Copyright © 2013 John Wiley & Sons, Ltd.     

Effect of alumina nanoparticles on the thermal properties of carbon fibre‐reinforced composites

In this work, we investigated the thermal behaviour of a carbon‐fibre composite impregnated with nano‐alumina‐based nanocomposites. First of all, we demonstrated that it is possible to obtain good dispersion and distribution of nanoparticles by mechanical mixing. In all the studied filler percentages, the presence of the ceramic filler did not affect the processability of the blends and the mechanical properties of the composites. First, the thermal stability of the nanocomposites was investigated by thermogravimetric analysis (TGA). Then, the fire reaction of the fibre‐reinforced composites was studied at different heat fluxes, by TGA, cone calorimeter and exposure to a direct flame. In presence of an oxidizing hyperthermal environment, the experimental data suggested the role of ceramic particles as anti‐oxidizer agent for the char and the carbon fibres. Moreover, the use of alumina nanoparticles allowed a slight reduction of heat release rate. Particularly at a heat flux of 35 kW/m², the burnt material containing the higher quantity of nano‐alumina maintained a residual structural integrity because of the higher presence of char that bound together the fibres. To estimate the integrity of the composites after exposure to a direct flame (heat flux 500 kW/m²), mechanical tests were carried out on the burnt specimens. Copyright © 2013 John Wiley & Sons, Ltd.     

Effects of variations in incident heat flux when using cone calorimeter test data for prediction of full‐scale heat release rates of polyurethane foam

The development of methods to predict full‐scale fire behaviour using small‐scale test data is of great interest to the fire community. This study evaluated the ability of one model, originally developed during the European Combustion Behaviour of Upholstered Furniture (CBUF) project, to predict heat release rates. Polyurethane foam specimens were tested in the furniture calorimeter using both centre and edge ignition locations. Input data were obtained using cone calorimeter tests and infrared video‐based flame area measurements. Two particular issues were investigated: how variations in incident heat flux in cone calorimeter tests impact heat release rate predictions, and the ability of the model to predict results for different foam thicknesses. Heat release rate predictions showed good agreement with experimental results, particularly during the growth phase of the fire. The model was more successful in predicting results for edge ignition tests than for centre ignition tests and in predicting results for thinner foams. Results indicated that because of sensitivity of the burning behaviour to foam specimen geometry and ignition location, a single incident heat flux could not be specified for generating input for the CBUF model. Potential methods to determine appropriate cone calorimeter input for various geometries and ignition locations are discussed. Copyright © 2014 John Wiley & Sons, Ltd.     

Fire retardancy of polypropylene/flax blends

A comprehensive characterization of the thermal and the fire behaviour is presented for polypropylene (PP) flax compounds containing ammonium polyphosphate (APP) and expandable graphite as fire retardants. Thermogravimetry coupled with an evolved gas analysis (TG-FTIR) was performed to ensure a significant thermal analysis. The fire response under forced flaming conditions was studied using a cone calorimeter. The external heat flux was varied between 30 and 70 kW m⁻² so that the results could be evaluated for different fire scenarios and tests. Different flammability tests (UL 94, limiting oxygen index, glow wire test, GMI 60261) were performed and the results compared with the cone calorimeter data. The different char forming mechanisms are described and the resulting fire retardancy is classified. The successful and ecological friendly fire retardancy is a technological breakthrough for PP/flax biocomposites.     

Study on Char Structure of Intumescent Flame-Retardant Polypropylene

The structure and properties of the char of intumescent flame retardant polypropylene (IFR-PP) have been studied by cone calorimeter, scanning electron microscope (SEM) and differential scanning calorimeter (DSC). Charring tendency analysis indicates IFR-PP is more likely to form a thick and homogenous char at low heat flux than that at higher heat fluxes. The SEM study indicates different char structures are formed at different stages. DSC analysis studies thermal stability of IFR-PP. Theoretical analysis of intuemscent charring shows when intumescent velocity increases, the heat diffusing into the underlying material will decrease if the thermal diffusivity of the material keeps constant.     

Flame retardation and thermal stability of novel phosphoramide/expandable graphite in rigid polyurethane foam

A novel flame retardant named diethylene N,N',N''‐tri (diethoxy)phosphoramide (DTP) was synthesized using diethyl phosphate and diethylenetriamine via Atherton–Todd reaction. Then, series of flame‐retardant water‐blown rigid polyurethane foams (RPUFs) with expandable graphite (EG) and DTP were prepared through box‐foaming. The results of thermogravimetric analysis showed that DTP/EG changed thermal degradation process of RPUF and promoted enhancing char residues. The complex flame‐retardant system (EG/DTP) endowed RPUF higher limiting oxygen index (LOI) values (29.1%–30.2%) and lower heat release rate peak (PHRR) values according to LOI and microscale combustion calorimeter tests. More importantly, the synergistic flame‐retardant effect between EG and DTP in RPUF was proved by the analysis of synergistic effectivity values. Based on the analysis of cone calorimetric tests, EG/DTP revealed remarkable effects to inhibit the fire intensity and smoke release of RPUF with decreased PHRR and total smoke production due to good char‐forming action. To further investigate the char‐residues of the foams after combustion, scanning electron microscope and energy dispersive X‐ray spectroscopy analyses were conducted. The results suggested that EG/DTP flame‐retardant system promoted RPUF forming a compact, continuous and phosphorus‐rich char layer as a good fire barrier in combustion. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46434.     

An effective intumescent flame retardancy of LDPE induced by the combination of APP and CNCO‐HA

A char‐forming agent poly(4,6‐dichloro‐N‐hydroxyethyl?1,3,5‐triazin‐2‐amine‐1,6‐diaminohexane) (CNCO‐HA) containing triazine rings was chosen for improving the flame retardant of low density polyethylene (LDPE). The synergistic effect of CNCO‐HA and Ammonium polyphosphate (APP) on the flame retardancy and char‐forming behavior of LDPE were investigated. The limited oxygen index (LOI) and vertical burning test (UL‐94) results indicated the optimal weight ratio of APP to CNCO‐HA was 3:1, and the LOI value of composite reached 31.0% with 30% intumescent flame retardant (IFR) loading. The cone calorimeter test analysis revealed that IFR presented excellent char forming and smoke suppression ability, and resulted in the efficient decrease of combustibility parameters. The thermogravimetric analysis results demonstrated that IFR reduced the thermal degradation rate at main stage of degradation. Scanning electron microscopy observed that IFR promoted to form a compact and continuous intumescent char layer. The Laser Raman spectroscopy spectra showed that larger graphitization degree was formed to enhance the strength of char, and Fourier transform infrared results presented that P‐O‐C and P‐O‐P structures in the residue char were formed to improve shield performance of the char layer to obtain better flame retardant properties of the composite. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43950.     

Influence of the pentaerythritol phosphate melamine salt content on the combustion and thermal decomposition process of intumescent flame‐retardant ethylene–vinyl acetate copolymer composites

Pentaerythritol phosphate melamine salt (PPMS) as a single‐molecule intumescent fire retardant was synthesized and characterized. The influence of the PPMS content on the combustion and thermal decomposition processes of intumescent‐flame‐retardant (IFR) ethylene–vinyl acetate copolymer (EVA) composites was studied by limiting oxygen index (LOI) measurement, UL 94 rating testing, cone calorimetry, thermogravimetric analysis, and scanning electron microscopy. The LOI and UL 94 rating results illustrate that PPMS used in EVA improved the flame retardancy of the EVA composites. The cone calorimetry test results show that the addition of PPMS significantly decreased the heat‐release rate, total heat release, and smoke‐production rate and enhanced the residual char fire performance of the EVA composites. The IFR–EVA3 composite showed the lowest heat‐release and smoke‐production rates and the highest char residue; this means that the IFR–EVA3 composite had the best flame retardancy. The thermogravimetry results show that the IFR–EVA composites had more residual char than pure EVA; the char residue yield increased with increasing PPMS content. The analysis results for the char residue structures also illustrated that the addition of PPMS into the EVA resin helped to enhance the fire properties of the char layer and improve the flame retardancy of the EVA composites. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42148.     

Fire Behavior of Natural Rubber Filled with Intumescent Flame Retardant Containing Graphite

Melamine salt of pentaerythritol phosphate/graphite (MPP‐G) mixture was prepared by dispersing graphite flakes in MPP during its synthesis. The chemical structure of MPP‐G was characterized by proton nuclear magnetic resonance, fourier‐transform infrared spectroscopy (FTIR), X‐ray diffraction (XRD), and scanning electron microscope. MPP‐G was blended with natural rubber (NR) at different loading levels and its effect on the thermal stability and flammability properties of NR was studied. The cone calorimeter results exhibited that the addition of MPP‐G to NR decreased the peak of heat release rate, mean heat release rate, total heat release, mean mass loss rate, mean effective heat of combustion, and maximum average rate of heat emission. Moreover, fire growth rate index and fire performance index values showed that NR/MPP‐G composites are safer than NR. The digital photographs of char formed after cone calorimeter test indicated the formation of a coherent char. The mechanism of flame retardation was studied based on FTIR, energy‐dispersive X‐ray spectrometry, and XRD analysis of char residue. J. VINYL ADDIT. TECHNOL., 26:155–164, 2020. © 2019 Society of Plastics Engineers     

Studies on intumescent flame retardant polypropylene composites based on biodegradable wheat straw

Wheat straw (WS) has numerous advantages compared with traditional bioadditives such as starch and lignin. So in this work, based on WS and silica microencapsulated ammonium polyphosphate, flame retardant polypropylene/wheat straw (WSP) composites were prepared by melted blend method. Flame retardant and thermal properties of WSP composites have been investigated. The results of cone calorimeter show that peaks of heat release rate and total heat release of the flame retardant WSP composite decrease substantially compared with those of pure polypropylene. The peak of heat release rate value of the flame retardant WSP composite decreases from 1290.5 to 247.9 kW/m², and the total heat release value decreases from 119.4 to 46.3 MJ/m². Meanwhile, thermal degradation and gas products of the flame retardant WSP composite were monitored by thermogravimetric analysis and thermogravimetric analysis‐infrared spectrometry. The result of thermal analysis shows that the flame retardant WSP composite has a high thermal stability and has a 30.0 wt% residual char at 600°C. From this work, we hope to provide a method to prepare flame retardant polymer composites with a biodegradable natural material‐WS.     

Application of cone calorimeter for the assessment of class of flame retardants for polypropylene

The study presented addresses the fire behaviour of polypropylene compounded with six classes of flame retardants. The application of cone calorimetry for the assessment of the thermal characteristics of the tested materials and their comparison with thermogravimetry are the central point of this research. This study only presents data for 25 kW/m² of incident heat flux exposure and includes five tests for polypropylene with no additives and five tests for polypropylene with flame retardants based on triglycidylisocyanurate and lignin. The data collected include the rate of heat release, mass loss rate, char yield, time to ignition and time of total combustion. Results represent meaningful comparison between the behaviour of the materials under simulated fire conditions, using the cone calorimeter, and in the slow dynamic environment utilized in thermogravimetric analysis. © 1998 John Wiley & Sons Ltd.     

Synthesis,characteristic of a novel flame retardant containing phosphorus and its application in poly(ethylene‐co‐vinyl acetate)

A novel flame retardant (SPDH) containing phosphorus was synthesized through the reaction of 10‐(2, 5‐dihydroxyphenyl)‐9, 10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO‐HQ) and synthesized intermediate product 3, 9‐dichloro‐2, 4, 8, 10‐tetraoxa‐3, 9‐diphosphaspiro(5.5)undecane‐3, 9‐dioxide (SPDPC). The structure and properties of SPDPC and SPDH were characterized by Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR) spectroscopy and thermogravimetric analysis (TGA). After blending with poly(ethylene‐co‐vinyl acetate) (EVA), the flame‐retardant properties of EVA/SPDH composites were estimated by cone calorimeter, limited oxygen index (LOI) and UL‐94 tests, whereas the thermal stabilities were investigated using TGA. The morphological microstructure of the char formed by EVA/SPDH composite after combustion in cone calorimeter was investigated by scanning electron microscopy (SEM). The results indicate that the flame retardant and thermal stability were improved by incorporation of SPDH. The rich foamy char layers were observed from the residues after combustion in a cone calorimeter, which exactly benefits the improvement of thermal stability and flame retardant property of materials. Copyright © 2010 John Wiley & Sons, Ltd.     

Preparation of aluminum hydroxide/aluminum phosphinate flame‐retardant poly(vinyl alcohol) foam through thermal processing

A novel flame‐retardant poly (vinyl alcohol) (PVA) composite foam was prepared successfully through thermal processing, which was filled with high content of flame retardant, based on aluminum hydroxide (ATH) and aluminum phosphinate (AlPi) and using water as plasticizer and blowing agent. The flame‐retardant property and mechanism of the prepared foam matrix were studied by vertical burning test, limiting oxygen index (LOI), cone calorimeter, scanning electronic microscopy (SEM) and X‐ray photoelectron spectroscopy (XPS). The experimental results showed that the PVA/ATH/AlPi (1/1.2/0.05) composite achieved LOI value of 41% and UL94 V‐0 (3.2 mm) rate. The addition of ATH and AlPi into PVA matrix significantly decreased flammability of the composites, because a more compact and continuous char layer of the PVA/ATH/AlPi composite could be formed, due to the involvement of AlPi in the char‐forming reaction. Compared with the pure PVA sample, the peak heat release rate (PHRR) and total heat release (THR) of PVA/ATH/AlPi (1/1.2/0.05) composite were reduced by 76.5% and 58.2%, respectively. Built upon this PVA‐based foam matrix with good flame retardancy, the flame‐retardant PVA‐based foam was successfully prepared through thermal extrusion. In addition, the influence of water content on melt viscosity, foam structure and mechanical strength was also analyzed. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42020.     

Thermal degradation and combustion behaviors of flame retarded glass fiber reinforced polyamide 6 composites based on cerium hypophosphite

In this work, cerium hypophosphite (CeHP) was synthesized and characterized by scanning electron microscope (SEM) and thermogravimetric analysis (TGA) test. CeHP presented rod‐like morphological feature with good thermal stability. Subsequently, CeHP was added into glass fiber reinforced polyamide 6 (GFPA) to develop flame retardant glass fiber reinforced polyamide 6 composites (FR‐GFPA). The flame retardancy of FR‐GFPA composites was characterized by limiting oxygen index (LOI), Underwriters Laboratories 94 testing (UL‐94), microscale combustion calorimeter, and cone calorimeter test. FR‐GFPA composite with 20 wt% CeHP loading passed UL‐94 V0 rating with a high LOI of 26.5 vol%. Cone Calorimeter test showed that peak of heat release rate (PHRR) and total heat release (THR) of FR‐GFPA composites were reduced 27.1% and 21.1% compared with those of GFPA. The mechanical measurement revealed that the tensile strength first increased and then decreased with the increase of CeHP loading. With 15 wt% CeHP loading, the tensile strength of FR‐GFPA composite was 43.0% higher than GFPA. TGA and char residue characterization revealed that the addition of CeHP could significantly promote the formation of condensed char residue. The FR‐GFPA composites obtained herein exhibited superior combined properties of fire resistance, thermal stability, and mechanical properties, demonstrating that CeHP will be a promising candidate for preparing high performance polyamide composites. POLYM. COMPOS., 37:3073–3082, 2016. © 2015 Society of Plastics Engineers     

Effect of curprous oxide in combination with molybdenum trioxide on smoke suppression in rigid poly(vinyl chloride)

Further investigation of the synergistic effect of smoke suppression between cuprous oxide and molybdenum trioxide in rigid poly(vinyl chloride) (PVC) was carried out by using a cone calorimeter (cone) at a high incident heat flux of 50 kW m^?2. Experimental data derived from the cone calorimeter indicated that binary mixtures of Cu₂O and MoO₃ clearly showed the synergistic effect in reducing smoke by decreasing total smoke production (TSP), average specific extinction area (av‐SEA), and smoke production rate (SPR). This result is in good agreement with that obtained from the NBS smoke chamber. However, the combustion process of rigid PVC could clearly be seen from the heat release rate (HRR), curve, SPR, and fire degradation obtained from the cone test, which could not be determined from the NBS smoke chamber. It was also found that the binary mixture showed the synergistic effect by increasing was also found that the binary mixture showed the synergistic effect by increasing char residue and reducing the fire degradation of the PVC backbone at a high incident heat flux of 50 kW.m^?2. All experimental data well supported the early cross‐linking mechanism of the PVC backbone mentioned in the literature and were consistent with the fire degradation behavior obtained from the cone calorimeter.     

Modeling and experimental studies of thermal degradation of glass fiber reinforced polymer composites

This study developed a numerical model that simulated the degradation rate and temperature profiles of a glass fiber reinforced polyester resin composite exposed to a constant heat flux in a cone calorimeter. By considering the thermal properties of the composite structure consisting of alternating layers of pure polymer and polymer‐infused glass fiber mat, the numerical model seeks to reproduce the experimental data from the cone calorimeter test. The final results are achieved through adding a simulated heat flux from the pilot ignition of the degraded gas of the polyester resin. The good agreement between the predicted and experimental results suggests that such models are cost‐saving tools over the process of designing and manufacturing of composites for meeting fire safety requirements, without having to fabricate many samples for testing and final selection. Copyright © 2013 John Wiley & Sons, Ltd.     

磷系阻燃剂FR/APP协效阻燃PP

采用氧指数测定仪、热重分析仪和锥形量热仪研究了磷系阻燃剂1,3,5-三(5,5-二甲基-1,3-二氧杂环己内磷酸基)苯(FR)和聚磷酸铵(APP)复配体系对聚丙烯(PP)材料阻燃性能的影响.结果表明,FR/APP提高了PP的极限氧指数(LOI)、热稳定性和残炭率,降低了热释放速率.当w(FR)为15%和w(APP)为10%复配阻燃PP时,复合材料的LOI为29.6%.阻燃级别达到UL 94 V-0级.     

Flame retardancy and thermal stability of polyhedral oligomeric silsesquioxane nanocomposites

The flame retardancy and thermal stability of polyhedral oligomeric silsesquioxane (POSS) nanocomposites are reviewed. Results are summarized and compared on the basis of structure–property relationships. Because of the variability of groups attached on POSS, they exhibit different performance in polymer nanocomposites: metal‐containing POSS show good catalytic charring ability; vinyl‐containing and phenyl‐containing POSS promote the strength of char. Improvements in the cone calorimeter (such as reduced peak heat release rate) are advantages of POSS as preceramics for fire retardancy compared with traditional flame retardants, and it will pave the way to the design of inorganic–organic hybrid polymer nanocomposites with enhanced flame retardancy and thermal stability. Copyright © 2011 John Wiley & Sons, Ltd.     

Application of a one‐dimensional thermal flame spread model on predicting the rate of heat release in the SBI test

A one‐dimensional thermal flame spread model was applied to predict the rate of heat release in the single burning item (SBI) test on the basis of the cone calorimeter data. The input parameters were selected according to the features of the SBI test and using particle board as a model tuning material. The features of the measured and calculated rate of heat release curves were compared for a series of 33 building products. The fire growth rate (FIGRA) indices were calculated to predict the classification in the forthcoming Euroclass system. The model gave correct classification for 90% of the products studied. An essential feature of the model is that only one cone calorimeter test at the exposure level of 50 kW m^?2 is needed. The model, therefore, provides a practical tool for product development and quality control. Copyright © 2001 John Wiley & Sons, Ltd.