Flame-retardant and thermal properties of highly efficient water-resistant intumescent flame-retardant polypropylene composites

Journal of Thermal Analysis and Calorimetry - The more efficient and hydrophobic modificated ammonium polyphosphate (M-APP) and charring agent (M-CA) were prepared based on sol–gel method,...     

Combustion properties and thermal degradation behavior of polylactide with an effective intumescent flame retardant

An intumescent flame retardant spirocyclic pentaerythritol bisphosphorate disphosphoryl melamine (SPDPM) has been synthesized and its structure was characterized by Fourier transformed infrared spectrometry (FTIR), ¹H and ³¹P nuclear magnetic resonances (NMR). A series of polylactide (PLA)-based flame retardant composites containing SPDPM were prepared by melt blending method. The combustion properties of PLA/SPDPM composites were evaluated through UL-94, limiting oxygen index (LOI) tests and microscale combustion calorimetry (MCC) experiments. It is found that SPDPM integrating acid, char and gas sources significantly improved the flame retardancy and anti-dripping performance of PLA. When 25 wt% flame retardant was added, the composites achieved UL-94 V0, and the LOI value was increased to 38. Thermogravimetric analysis (TGA) showed that the weight loss rate of PLA was decreased by introduction of SPDPM. In addition, the thermal degradation process and possible flame retardant mechanism of PLA composites with SPDPM were analyzed by in situ FTIR.     

The influence of organo-modified sepiolite on the flame-retardant and thermal properties of intumescent flame-retardant polylactide composites

Polylactide (PLA) composites based on intumescent flame-retardant (IFR) and organo-modified sepiolite (OSEP) were prepared via direct melt compounding. The uniform dispersion of OSEP in the PLA matrix was observed by TEM, but some agglomerates still existed at the high loading. Tensile results showed that high loading of the conventional IFR led to a reduction in tensile strength of PLA composites; however, replacing a portion of the IFR with modified sepiolite in the PLA matrix improved this result. The thermal degradation temperature of the PLA/IFR/OSEP composites determined by thermogravimetric analysis was lower than that of neat PLA, as a consequence of the catalyzed carbonization induced by the addition of IFR and OSEP. The formulation with 13 mass% IFR and 2 mass% OSEP exhibited the highest LOI value of 32 vol% and also reached UL-94 V-0 rating in the vertical burning tests. Furthermore, the co-addition of IFR and OSEP gave rise to a significant reduction in peak heat release rate (PHRR) and total heat release (THR) of PLA composites during combustion, particularly in the case of PLA/IFR13/OSEP2 (82% reduction in PHRR and 69% in THR). The excellent fire resistance of PLA/IFR13/OSEP2 could be attributed to that IFR catalyzed carbonization of PLA to form the char, while OSEP resulted in further stabilization in the charred layers.     

The influence of soda additive on the thermal properties of red mud

The dehydration and decomposition of the red mud from Seydięehir Aluminum factory, mixed with soda were investigated under dynamic and isothermal conditions. Soda was added to the red mud samples as much as 50, 100 and 150 mass% of Na₂CO₃ of the red mud sample's mass. To determine the effect of soda additive on the red mud's thermal properties, using TG and DTA techniques simultaneously under atmospheric conditions. Furthermore, the original red mud sample's XRD and IR spectrum curves were investigated. It seems that the temperatures of the endothermic peaks of the red mud decreased with the amount of soda added. However the endothermic peak's temperature readings showed that the melting of soda increased gradually with the quantity of soda used. This revised version was published online in July 2006 with corrections to the Cover Date.     

Manufacturing,thermal stability,and flammability properties of polypropylene containing new single molecule intumescent flame retardant

Melamine salt of pentaerythritol phosphate kaolin (MPPK) was synthesized by the reaction of pentaerythritol phosphate with kaolin (K) and melamine. The structure of MPPK was confirmed by EDXS, ¹H NMR, FTIR, and XRD. MPPK was blended with polypropylene (PP) at different loading levels. Thermogravimetric analysis (TGA) results showed that MPPK improved the thermal stability of PP at high temperatures in all PP composites. Vertical burning rate test manifested that PP composites can achieve V0 at 20% and 25% MPPK loading levels. Cone calorimeter data exhibited that addition of 25% MPPK to PP reduced peak of heat release rate (pHRR) and total heat release (THR) by 86% and 76% and increased the char residue after test to 67%. The results of PP/25% MPPK composite were compared with the data obtained from PP containing 25% K and 25% of traditional intumescent flame retardant composed of melamine phosphate (MP), pentaerythritol (PE), and K. The outcomes indicated that MPPK was more efficient in flame retardancy than the other systems. The digital photographs and SEM images for char residue demonstrated that MPPK succeeded in forming cellular and coherent char layer on the PP surface. The main advantage of adding 25% MPPK to PP was its ability to preserve nearly the inner half of the sample without burning after cone calorimeter test.     

Kinetic analysis of the thermal degradation of an epoxy-based intumescent coating

The aim of this work is to analyse and to simulate the kinetics of pyrolysis of an intumescent formulation designed to protect steel in the case of hydrocarbon and jet fires. The coating is based on a thermoset epoxy-amine resin system into which two fire retardant agents, boric acid and ammonium polyphosphate derivative have been incorporated. Industrial tests (jet fire tests) are usually used to evaluate the degradation mode of an intumescent coating. But these tests are quite expensive, and as the heating rates are extremely high (between 500 and 800 °C/min), it is not possible to evaluate the thermal degradation behaviour of the intumescent coating directly by thermogravimetric analyses. That is why it is necessary to develop predictive models of kinetics of degradation of these intumescent coatings. In this work, the coating has been pyrolyzed at different heating rates and a predictive model of its kinetics of degradation has been developed.     

Modified montmorillonite combined with intumescent flame retardants on the flame retardancy and thermal stability properties of unsaturated polyester resins

Modified montmorillonite‐containing phytic acid (PA‐MMT) has been prepared by acid treatment and then introduced into unsaturated polyester resin (UPR) with an intumescent flame retardant (IFRs). The flame retardancy and thermal degradation of UPR/IFRs/PA‐MMT were evaluated by a limiting oxygen index (LOI) test, a vertical burning test (UL‐94), a thermogravimetric analysis (TGA), and a cone calorimeter test (CCT). Besides, the mechanical properties were studied by a universal testing machine. The LOI value of UPR/IFRs/PA‐MMT composites was increased to 29.2%. The CCT results indicated that the incorporation of PA‐MMT and IFRs significantly improved the combustion behavior of UPR. The results of the mechanical properties indicated that 1.5 wt% loading of PA‐MMT in UPR/IFRs showed the highest improvement in flexural strength and tensile strength. The flame‐retardant mechanism of PA‐MMT/IFRs was examined and discussed based on the results of combustion behavior and char analysis.     

Flame retardancy and thermal degradation of intumescent flame retardant polypropylene material

The flame retardancy and thermal degradation properties of polypropylene (PP) containing intumescent flame retardant additives, i.e. melamine pyrophosphate (MPyP) and charring‐foaming agent (CFA) were characterized by limiting oxygen index (LOI), UL 94, cone calorimeter, microscale combustion calorimetry, and thermogravimetric analysis (TGA). It has been found that the PP material containing only MPyP does not show good flame retardancy even at 30% additive level. Compared with the PP/MPyP binary system, the LOI values of the PP/MPyP/CFA ternary materials at the same additive loading are all increased, and UL 94 rating is raised to V‐0 from no rating (PP/MPyP). The cone calorimeter results show that the heat release rate and mass loss rate of some ternary materials decrease in comparison with the binary material. The microscale combustion calorimetry results indicate that the sample containing 22.5 wt% MPyP and 7.5 wt% CFA has the lowest heat release rate among all samples. The TGA results show that the thermal stability of the materials increases with the addition of MPyP, while decreases with the addition of CFA. Copyright © 2009 John Wiley & Sons, Ltd.     

Synergistic effect of nanoflaky manganese phosphate on thermal degradation and flame retardant properties of intumescent flame retardant polypropylene system

Nanoflaky manganese phosphate (NMP) was synthesized from manganese nitrate and trisodium phosphate dodecahydrate, and used as a synergistic agent on the flame retardancy of polypropylene (PP)/intumescent flame retardant (IFR) system. The thermogravimetric analysis (TGA), real time Fourier-transform infrared (RTFTIR) spectroscopy measurements, cone calorimeter (CONE) and microscale combustion calorimeter (MCC) were used to evaluate the synergistic effects of NMP on PP/IFR system. When IFR + NMP was fixed at 20 wt% in flame retardant PP system, the TGA tests showed that NMP could enhance the thermal stability of PP/IFR system at initial temperature from about room temperature to 440 °C and effectively increase the char residue formation. The RTFTIR results revealed that NMP could clearly change the decomposition behavior of PP in PP/IFR system, which promotes decomposition at the initial temperature from about room temperature to 260 °C and forms more effective barrier layer to protect PP from decomposing at high temperature from about 260 °C to 500 °C. The CONE tests indicated that the addition of NMP in PP/IFR system not only reduced the peak heat release rate (HRR), but also prolonged the ignition time. The MCC results revealed that PP/IFR/NMP system generated less combustion heat over the course of heating than that of PP/IFR system. And scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) were used to explore the char residues of the PP/IFR systems with and without NMP.     

Synergistic effect of zeolite 4A on thermal,mechanical and flame retardant properties of intumescent flame retardant HDPE composites

The combination of synergistic agent with intumescent flame retardant (IFR) systems provides a promising way to prepare high performance IFR composites. In this study, the effects of the synthetic zeolite 4 A in combination with the IFR system consisting of ammonium polyphosphate (APP) and tris (2-hydroxyethyl) isocynurate (THEIC) on thermal degradation, mechanical properties, flame retardancy and char formation of high-density polyethylene composites were investigated by limiting oxygen index (LOI) measurement, cone calorimetry, scanning electron microscopy and laser Raman spectroscopy. The LOI value of HD/FR/Z-0.5 composite with an optimum content of 0.5 wt. % zeolite 4 A and 25 wt. % of total flame retardant reaches 26.3 %. A low loading of zeolite 4 A can improve the bench-scale combustion performance as determined by cone calorimetry, and promote the formation of more compact char residue with a highly graphitic structure. However, a low loading of zeolite in combination with the IFR system consisting of APP and THEIC produces no significant changes in mechanical performance.     

Influence of layered zinc hydroxide nitrate on thermal properties of paraffin/intumescent flame retardant as a phase change material

The thermal properties of paraffin as phase change material (PCM), combined with layered zinc hydroxide nitrate (LZHN) and intumescent flame retardant (IFR), have been studied by thermogravimetric analysis (TG), TG-Fourier transform infrared spectrometry (TG-FTIR), cone calorimeter (CONE),and differential scanning calorimetry (DSC). The TG results indicated that the thermal stabilities of the paraffin and paraffin/IFR composites could be improved when dodecyl sodium sulfate-modified LZHN (ds-LZHN) was incorporated. The TG-FTIR results indicated that ds-LZHN could reduce the release of combustible gases for paraffin and paraffin/IFR. The CONE results showed that the flame-retardant efficiency of IFR could be improved in the paraffin/IFR system owing to ds-LZHN. DSC results presented that the phase change temperatures and latent heats of the composites were determined by the dispersed paraffin with their mass percentage.     

Study of thermal properties of thallium hexavanadate

A DTA study of the thermal properties of Tl₂V₆O₁₆, showed that its structure is not decomposed up to 475 °C. It melts at 505 °C. Tl₂V₈O₂₁ and Tl₃V₅O₁₄ crystallize successively from the melt.     

TG-MS and TG-FTIR applied for an unambiguous thermal analysis of intumescent coatings

Thermogravimetry (TG), thermogravimetry coupled with mass spectroscopy (TG-MS) and thermogravimetry coupled with Fourier transform infrared spectroscopy (TG-FTIR) were used to characterise the thermo-oxidative behaviour of two intumescent coating materials. The temperature dependence, the corresponding volatile products and the amount of residue of the different processes were determined. Using both TG-MS and TG-FTIR results in an unambiguous interpretation of the volatile products. Characteristics such as the influence of endothermic reactions, the release of non-flammable gases, the dehydrogenation enhancing the char formation and the stability of the cellular char were discussed in detail. It was demonstrated, that TG, TG-MS and TG-FTIR are powerful methods to investigate mechanisms in intumescent coatings and that they are suitable methods in respect to quality assurance and unambiguous identification of such materials. This revised version was published online in July 2006 with corrections to the Cover Date.     

Synthesis and thermal stability of a novel phosphorus-nitrogen containing intumescent flame retardant

A novel phosphorus-nitrogen containing intumescent flame retardant （P-N IFR） was prepared via the reaction of dichlor-opentate with N-methylaniline. The structure of the product was confirmed by ^1H NMR, ^31p NMR, MS and IR. TGA analysis showed it has effective thermal stability.     

Study of thermal properties of endellite clay compound

The temperature dependence of the thermal properties (specific heat,C _p, thermal diffusivity,a, and thermal conductivity,K) of endellite clay has been investigated over the temperature rangeR·TT/280 °C using the plane temperature wave technique. The experimental results showed that in the initial stage of temperature rise botha andK diminish exponentially with increasing temperature up to 100 °C. Above 100 °C, the thermal parameters are found to reach stable values, namely,C _p=0.22±0.008 cal g^–1 deg^–1,a=(5.0±0.18)–10^–4 cm² sec^{– 1} andK=(2.2±0.16) · 10^–4 cal cm^–1 sec^–1 deg^–1. The explanation of the results was supported by using DTA and TG analysis.

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Zusammenfassung In einem Temperaturbereich zwischen Raumtemperatur und 280 °C wurde die Temperaturabhängigkeit der thermischen Eigenschaften (spezifische WärmeC _p, Temperaturleitfähigkeita, WärmeleitfähigkeitK) von Endellittonerde untersucht. Die Ergebnisse zeigen, daß sowohla als suchK im ersten Abschnitt der Temperaturzunahme mit steigender Temperatur bis 100 °C exponentiell abnehmen. Oberhalb 100 °C erreichen die Parameter stabile Werte:C _p=0,22 ±0,008 cal g^–1 deg^–1,a=(5,0±0,18)·10^–4 cm² sec^–1 undK=(2,2±0,16)·10^–4 cal cm^–1 sec^–1 deg^–1. Die Erklärung der Ergebnisse wurde unter Zuhilfenahme von DTA und TG durchgeführt.

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( _p, ) T280°. , 100° K . 100° _n=,22 ±0,008 · ^–1· ^–1, =5,0±0,18·10^{–4 2}· ^–1 K=2,2±0,16· 10^–4 · ^–1· ^–1· ^–1. .

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We wish to thank Dr. N. Afify, Phys. Dept. Assiut University, for his assistance during DTA and TGA analysis.     

Influence of thermophysical properties on burning behavior of intumescent fire-retardant materials

Thermophysical properties of intumescent fire-retardant (IFR) materials are important parameters as input data in modeling the combustion process of IFR materials in a fire. In this paper, the influences of several thermophysical properties on burning behavior of IFR materials are simulated based on a combustion model of IFR materials. Thermophysical properties selected here are thermal conductivity of virgin material and char layer, specific heat capacity of virgin material, density of virgin material, surface emissivity of virgin material and char layer, heat of decomposition, heat of combustion, and intumescent temperature. Predicted heat release rates curves for the IFR material at an incident heat flux of 50 kW m^?2 are shown for the varied thermophysical parameters’ values. The results show that these varied parameter values can affect the burning behavior of materials remarkably. A comparison with experimental results demonstrates that the predictions of heat release rates are in reasonably good agreement with the experiment.     

Preparation and expansion properties of a novel UV-curable intumescent flame-retardant coating

Journal of Thermal Analysis and Calorimetry - N,N′-bis(2,4-di(acryloyloxyethyl)-[1,3,5]-triazin-2-yl)-hexane-1,6-diamine(BDAETH) and 2,2-dimethyl-1,3-propanediol glycerol-methacrylate...