Influence of external heat flux and coating thickness on the thermal insulation properties of two different intumescent coatings using cone calorimeter and numerical analysis

Polymeric intumescent coatings are fire protective materials that increase their thermal resistance when exposed to high temperatures to prevent building structures from damage. The idea of the investigation was to develop a simple test method to determine the time dependent thermal conductivity of intumescent coatings. Therefore steel plates were coated with two different intumescent systems. During cone calorimeter tests the temperature at the back side of the coated plates was measured. These results were used to calculate the time dependent thermal resistance of the protective layer with the simulation program IOPT2D for different external heat fluxes and different layer thickness. Copyright © 2003 John Wiley & Sons, Ltd.     

Fire‐resistant effect of nanoclay on intumescent nanocomposite coatings

The aim of the study is the development of an intumescent nanocomposite coating to provide fire protection for the metallic substrate. Acrylic nanocomposites containing nanoclay and relative intumescent nanocoatings are prepared. The effect of nanoclay on the thermal degradation of an intumescent nanocomposite coating is analyzed by using differential thermal analysis, thermogravimetry, and X‐ray diffraction. The influence of the added content of nanoclay on fire performance is studied by a fire protection test and measurements of the limiting oxygen index and effective thermal conductivity. The distribution of nanoparticles in the acrylic nanocomposite is characterized by transmission electron microscopy. The flame‐retardant efficiency of the intumescent nanocomposite coating is improved by 1.5% well‐distributed nanoclay particles. However, 3% nanoclay produces a negative effect on the fire performance of the coating. Fire protection tests and scanning electron microscopy observations reveal that the fire‐retardant property of a conventional intumescent coating is destroyed by aging, whereas the nanocomposite coating modified with 1.5% nanoclay demonstrates good aging and fire resistance. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 1681–1689, 2007     

Development of fire‐retarded materials—Interpretation of cone calorimeter data

There is little consensus within the fire science community on interpretation of cone calorimeter data, but there is a significant need to screen new flammability modified materials using the cone calorimeter. This article is the result of several discussions aiming to provide guidance in the use and interpretation of cone calorimetry for those directly involved with such measurements. This guidance is essentially empirical, and is not intended to replace the comprehensive scientific studies that already exist. The guidance discusses the fire scenario with respect to applied heat flux, length scale, temperature, ventilation, anaerobic pyrolysis and set‐up represented by the cone calorimeter. The fire properties measured in the cone calorimeter are discussed, including heat release rate and its peak, the mass loss and char yield, effective heat of combustion and combustion efficiency, time to ignition and CO and smoke production together with deduced quantities such as FIGRA and MARHE. Special comments are made on the use of the cone calorimeter relating to sample thickness, textiles, foams and intumescent materials, and the distance of the cone heater from the sample surface. Finally, the relationship between cone calorimetry data and other tests is discussed. Copyright © 2007 John Wiley & Sons, Ltd.     

Effects of natural weathering on the fire properties of intumescent fire‐retardant coatings

Fire‐retardant coatings could be one option for providing enhanced protection to buildings during a wildfire, particularly when applied to combustible siding and in under‐eave areas. Limited studies have been conducted on their effectiveness but maintaining adequate performance after weathering has been questioned. This paper reports on a study evaluating the effect of natural weathering on the performance of intumescent‐type fire‐retardant coatings. The main concerns were (a) the reduction of ignition resistance of the coating after weathering and (b) the coating might contribute as a combustible fuel and assist the fire growth after weathering. This study evaluated the performance of 3 intumescent coatings that were exposed to natural weathering conditions for up to 12 months. A bench‐scale evaluation using a cone calorimeter was used to evaluate the performance of the coatings at 3 heat flux levels (30, 50, and 70 kW/m²). Our results showed that weathering exposure reduced the effectiveness of fire protection of intumescent coatings, but the weathered coatings did not act as additional fuels. Weathering orientation showed much less effect on the performance of intumescent coatings in comparison to other parameters. There was statistical evidence that weathering duration, heat flux level, and coating type affected the combustion properties.     

Characterization of highly under‐ventilated fires using the cone calorimeter

The cone calorimeter, originally designed with an ‘open configuration‘, may be used in combination with a closed‐combustion chamber in order to test specimens in oxygen‐depleted atmospheres (air vitiation effect) or in fuel‐rich combustion (ventilation effect). However, highly under‐ventilated conditions are not achievable, as a consequence of an overconsumption of oxygen due to the incomplete confinement of the flame and imperfections in the air tightness of the combustion volume. In this work, these issues were solved by lowering the combustion zone, in order to fit a 600 mm chimney on the top of the controlled‐atmosphere chamber, and further improving the sealing of the whole setup. n‐Heptane was used as a reference fuel, and its combustion properties were determined in under‐ventilated conditions. The yields of main combustion species correlated well with the global equivalence ratio, for values of Φ up to three. The use of a Fourier‐transform infrared spectrometer allowed further refinement of the total unburned‐fraction composition. The relative concentration of species like methane, ethylene, or acetylene was shown to be relatively constant over the range of under‐ventilated conditions. Copyright © 2015 John Wiley & Sons, Ltd.     

Assessing the reaction to fire of cables by a new bench‐scale method

The recently approved EU Construction Products Regulation (CPR) applies to cables as construction products. The difficulty of predicting the fire performance of cables with respect to propagation of flame and contribution to fire hazards is well known. The new standard EN 50399 describes a full‐scale test method for the classification of vertically mounted bunched cables according to CPR. Consideration of the material, time, and thus cost requires an alternative bench‐scale fire test, which finds strong demand for screening and development purposes. The development of such a bench‐scale fire test to assess the fire performance of multiple vertically mounted cables is described. A practical module for the cone calorimeter is proposed, simulating the fire scenario of the EN 50399 on the bench scale. The efficacy of this module in predicting full‐scale CPR test results is shown for a set of 20 different optical cables. Key properties such as peak heat release rate (PHRR), fire growth rate (FIGRA), and flame spread are linked to each other by factors of around 5. In a case study, the bench‐scale test designed was used to investigate the influence of the main components on the fire behaviour of a complex optical cable. Copyright © 2016 John Wiley & Sons, Ltd.     

Enhanced flame-retardant performance of rigid polyurethane foam by using APTES-MMT and ATH mixed intumescent coatings

The design of environment-friendly fireproof rigid polyurethane foams (RPUFs) that completely prevent ignition or the spread of fires is important for energy conservation and emission reductions. In this paper, an intumescent flame-retardant coating was prepared and coated onto the surface of a RPUF to improve its flame retardancy. Vertical combustion experiments (UL-94) showed that, compared with the pure RPUF, a RPUF coated with the expansion coating successfully self-extinguished without a droplet formed after ignitor removal. Thermogravimetric analyses showed that the expanded coating effectively increased the rate of carbon residue formation. Cone calorimetry showed that when the pigment-to-binder ratio was 3.5:1, with 5% modified montmorillonite, 6% aluminum hydroxide, and 4% titanium dioxide, the intumescent coating effectively reduced the heat release rate and total heat release of the RPUF. Remarkably, the smoke release rate and total exhaust gas volume showed that the expanded coating provided obviously enhanced smoke suppression. Therefore, the flame retardancy and toxic smoke suppression provided by the RPUF thermal insulation material is essential and very useful for healthy development of human society and the environment.     

Investigation of fire behavior of rigid polyurethane foams containing fly ash and intumescent flame retardant by using a cone calorimeter

Cone calorimeter is one of the most useful bench‐scale equipment which can simulate real‐world fire conditions. Therefore, cone calorimeter tests have been the most important and widely used tests for research and development of fire behavior of polymeric materials. In this study, fire behavior of rigid polyurethane foams containing fly ash (up to 5 wt %) and intumescent flame retardant (up to 5 wt %) composed of ammonium polyphosphate/pentaerythritol was investigated by using a cone calorimeter. In addition, thermogravimetric analysis of the additives and the foams were also carried out to explain the effects of fly ash and intumescent flame retardant on fire behavior of the foams. Experimental results indicated that rigid polyurethane foam containing fly ash and the intumescent flame retardant in comparison with pure rigid polyurethane foam shows significantly enhanced fire resistance and thermal stability. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Comparative study of the fire protection performance and thermal stability of intumescent fire-retardant coatings filled with three types of clay nano-fillers

The fire protection and thermal stability properties of intumescent fire-retardant coatings filled with three various clay nano-fillers (layer double hydroxide [LDH], montmorillonite [MMT], and sepiolite) were compared by fire protection tests and thermo-gravimetric analysis. The fire protection tests show that the incorporation of three fillers improves the fire protection properties of the intumescent fire-retardant coatings and the addition of 1 wt% sepiolite exhibits the lowest flame spread rating of 9.9 and equilibrium backside temperature of 164.5°C at 900 seconds. TG analysis shows that the incorporation of nano-fillers imparts a considerable enhancement of thermal stability and char formation to the intumescent coatings. Especially, the coating with 1 wt% sepiolite acquires the highest residual weight of 34.2% among the samples. Char residue analysis presents that the introduction of clay nano-fillers plays a positive role in enhancing the compactness and anti-oxidation ability of the char residues, and this positive effect as well as the flame-retardant efficiency depends on the types of clay nano-fillers. The three types of layered clay nano-fillers exhibit synergistic flame-retardant effectiveness in the order of sepiolite > MMT > LDH.     

Linking the flame‐retardant mechanisms of an ethylene‐acrylate copolymer,chalk and silicone elastomer system with its intumescent behaviour

In this paper the flame‐retardant mechanisms of a flame‐retardant system consisting of ethylene‐acrylate copolymer, chalk and silicone elastomer are linked to its foaming process and to its formation of a final intumescent structure. Thermocouples were placed inside and at the surface of cone calorimeter test specimens in order to measure the temperature at different depths during the formation of the intumescent structure. The temperature and visual observations of the foaming process were then linked to chemical reactions seen with thermogravimetric analysis and also coupled with earlier knowledge of the flame‐retardant mechanism. A correlation is seen between the chemical reactions, the temperature (inside and at the surface of a cone calorimeter test specimen) as measured by thermocouples and visual observations in the intumescent process. Further, the outcome of this study provides useful information for achieving a deeper understanding of the flame‐retardant mechanisms of the ethylene‐acrylate copolymer, chalk and silicone elastomer system. Copyright © 2005 John Wiley & Sons, Ltd.     

A mechanistic study of the fire performance of the silica and zinc borate nanoparticles-incorporated intumescent coatings based on epoxy resin

An epoxy-based intumescent coating containing the silica and zinc borate nanoparticles was fabricated. The fire performance of the coating with the optimum formulation was investigated in terms of the changes in the physical and chemical structure of the formed char layer during the exposure to a temperature of 1000°C. The state of the chemical structure was analyzed by performing the Fourier-transform infrared spectroscopy, x-ray diffraction, and x-ray photoelectron spectroscopy analysis from the char layer at the three-time intervals of 10, 30, and 60 min of the heating process. The innovative Condorcet method was also employed to examine the changes in the physical structure of the formed char layer. Some instabilities were detected in the physical structure of the char layer in the middle period of heating. Moreover, a gradual formation of silicon carbide crystalline structure was observed on top of the surface, followed by its oxidation to silica over time. In contrast, in the bulk structure, silicon crystalline structures (Coesite) intensified with time. Boron nitride was also increasingly created on the top surface and in the bulk of the coating over the heating time. These findings proved the effective role of the silica and zinc-borate nanoparticles in the fire performance of epoxy-based intumescent coatings.     

Numerical simulations of a full‐scale cable tray fire using small‐scale test data

This paper presents a computational fluid dynamics (CFD)‐based modeling strategy for the prediction of cable tray fire development. The methodology is applied to a set of five horizontal trays (each 2.4‐m long and 0.45‐m wide) that are positioned with a 0.3‐m vertical spacing and set up against an insulated wall. Each tray contains 49 power PVC cables. Ignition is performed with an 80‐kW propane burner centrally positioned at 0.2 m below the lowest tray. A collection of four groups of cables per tray (made of one homogeneous material) is considered. These groups are separated by longitudinal slots of air to “mimic” their relatively “loose arrangement.” The thermal properties and surface ignition temperature are estimated from cone calorimetry (CC). When the ignition temperature is reached, the cables burn according to a prescribed heat release rate per unit area (HRRPUA) profile obtained from CC, as is or in a modified shape. A realistic flame pattern is predicted. Furthermore, using only data from CC, the peak HRR is underpredicted, and the time to reach the peak is overpredicted. The proposed “design” for the modified HRRPUA CC‐profile significantly improves the results.     

Flame retardancy and crack resistance of transparent intumescent fire‐resistive coatings

In this article, dihydroxy polydimethylsiloxane (n = 5–10) was introduced into the structure of polyphosphate (PPE) to get siloxane‐modified polyphosphate (SiPPE). Five kinds of SiPPEs with different Si contents were obtained. FTIR (Fourier Transform Infrared spectroscopy) ICP (Inductively Coupled Plasma Emission Spectroscopy), ³¹P NMR (Nuclear Magnetic Resonance Spectroscopy) and TGA (Thermogravimetric Analysis) were used to characterize the composition and structure of PPE and SiPPEs. Six kinds of transparent fire‐resistive coatings were prepared by the mixing of amino resin with PPE and five kinds of SiPPEs. The results of the fire protection test showed that both the fire‐resistive time of coatings and intumescent factor of char layers increased with the increase in content of Si. The results of TGA demonstrated that the carbonaceous residue of coating also increased regularly. The hardness, flexibility, digital photos, SEM (Scanning Electronic Microscopy) and other testing results showed that the introduction of silicon oxygen segment can effectively improve the crack resistance. The charcoal layer structure was more solid than before and collapse was not obvious after long time flame shock. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42423.     

Experimental and numerical study of burning behaviors of flaxboard with intumescent coating and nanoparticles in the cone calorimeter and single burning item tests

This paper presents an experimental and numerical investigation of the effects of intumescent coating and nanoparticles on the burning behaviors of flaxboard. Virgin flaxboard samples and those coated with intumescent coatings (with/without nanoparticles) were tested in the cone calorimeter and single burning item (SBI) test. Experimental results show a significant increase in the time to ignition and also a reduction in the heat release rate by the intumescent coatings. In order to explain quantitatively and predict the effects of the intumescent coating, a global fractional factor (the ratio of the heat flux at the interface of the intumescent surface and the char layer of flaxboard to the surface heat flux when there is no intumescent coating layer) was introduced based on analytical solutions for charring materials. The fractional factor for the intumescent coatings was found by comparing predictions to the experimental data in the cone calorimeter test and, subsequently, was incorporated in an upward flame spread model, along with the ignition and thermal properties deduced from the ignition tests, to predict the burning rates in the SBI tests. Copyright © 2011 John Wiley & Sons, Ltd.     

Smoke suppression properties of epoxy crosslinked structure and intumescent fire retardant in epoxy‐based intumescent fire‐retardant coating

In this article, the smoke production behaviors of crosslinked epoxy/polyamide resin (EP/PA) and intumescent fire retardant (IFR) in epoxy‐based intumescent fire‐retardant coating (IFR‐EP) have been investigated using cone calorimeter, smoke density instrument, and thermogravimetric analysis and Fourier transform infrared spectroscopic measurement. The static and dynamic smoke production behaviors of EP/PA and IFR‐EP indicate that the IFR has an excellent smoke suppression effect on EP/PA by forming protective char layer in the late combustion stage, while the epoxy crosslinked structure in IFR‐EP can enhance the thermal stability and reduce smoke production in the early combustion stage. In addition, according to the discussion of pyrolysis gas products, the IFR can effectively suppress the production of toxic and inflammable gases during the combustion process. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43912.     

Methane calibration burner and C‐factor determination with cone calorimeter – validation of the standardized calibration protocol

The cone calorimeter is one of the major fire tests. In its reference standard ISO 5660‐1, the apparatus (and especially a characteristic of its orifice plate mass flow meter, called C‐Factor) is calibrated using a methane burner set at 5 kW. However, measurements performed in end‐use are in the range 1–10 kW. In addition, standard proposes to check linearity at 1 and 3 kW, which means in the lowest part of the range. This communication establishes the validation of the linearity on the whole range and determines the optimal condition for C‐factor determination. It justifies the technical choices of the standard. Copyright © 2014 John Wiley & Sons, Ltd.     

The calculation of the heat release rate by oxygen consumption in a controlled‐atmosphere cone calorimeter

The standard cone calorimeter according to ASTM E 1354 and ISO 5660 enables reaction‐to‐fire tests to be performed in ambient atmospheric conditions. A controlled‐atmosphere chamber modifies the standard apparatus in a way that allows tests to be performed in nonambient conditions as well. The enclosed chamber is placed underneath the standard exhaust hood and does not have a closed connection to the hood. With this open arrangement, the exhaust gases are diluted by excess air drawn in from the laboratory surroundings. Heat‐induced changes in the consequential dilution ratio affect the calculation of fire quantities and, when neglected, lead to deviations of up to 30% in heat release rate. The paper introduces a test protocol and equations to calculate the heat release rate taking dilution effects into account. A mathematical correction is shown that compensates for the dilution effects while avoiding extensive mechanical changes in the equipment. Copyright © 2013 John Wiley & Sons, Ltd.     

Effects of inorganic fillers on the shear viscosity and fire retardant performance of waterborne intumescent coatings

In the present work, the effects of inorganic fillers on the fire retardant performance of waterborne intumescent coatings are investigated by thermogravimetry (TG), capillary rheometer, X-ray diffraction spectroscopy (XRD) and fire retardant test, etc. The TG results indicate that the thermal stability of vinyl acetate-vinyl ester of versatic acid copolymer (hereafter VAc-VeoVa) in VAc-VeoVa/Si–Al powder composite or in VAc-VeoVa/Halloysite nanometer-tube (HNTs) composite is improved mainly due to the release of the crystal water in Si–Al powder or HNTs. Capillary rheometer analysis results demonstrate that the VAc-VeoVa/HNTs composite melt possesses the highest shear viscosity, because of the large specific surface area of HNTs and the strong interaction force between HNTs and VAc-VeoVa. Weight loss difference (ΔT) of filler/ammonium polyphosphate (APP) composites show antagonism effects at 300 °C < T < 650 °C and synergistic effects at T > 650 °C. The fire retardant test results show the coatings using TiO₂/Si–Al powder/HNTs (8/1/1) as multiple fillers obtains an intumescent char layer with intumescent ratio of 28.14 and presents excellent fire retardant performance (3327 s). It is found that the high melt viscosity, resulted from the effect of inorganic filler, immobilizes the relaxation and rotation of polymer chain, restricts the intumescent behavior of the coatings, which leads to the formation of an intumescent char layer with lower intumescent ratio and the shortening of the fire retardant time. Moreover, the antagonism effect between filler and APP reduces the catalytic dehydration efficiency of pentaerythritol (PER) and VAc-VeoVa, which, as a result, also affects the final fire retardant performance of coatings.     

Use of epoxy–phenolic lacquers in food can coatings: Characterization of lacquers and cured films

Liquid and cured epoxy–phenolic lacquers used as can coatings were characterized. Tinplate was used as the base material, which was coated with lacquers of different epoxy to phenolic ratios (EPRs) from a commercial source. Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA) were used together to obtain helpful information about the degree of curing and the composition of the lacquers. From FTIR analysis, we were able to infer that the lacquers were composed of a high‐molecular‐weight diglycidyl ether of bisphenol A type epoxy resin and a resol‐type phenolic resin. In addition, from FTIR spectra, we estimated the EPRs of lacquers applied on the tinplate and detected if they had been overcured. The EPRs of the applied lacquers were estimated also from DSC analysis. From TGA, we detected undercuring in the applied lacquers. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 95: 1448–1458, 2005     

Effect of expandable graphite and ammonium polyphosphate on the thermal degradation and weathering of intumescent fire-retardant coating

This research aims to study the effect of ammonium polyphosphate and expandable graphite on the intumescent coating formulations (ICF). The coating presented in this research article is based on carbon source expandable graphite (EG), blowing agent melamine, acid source ammonium polyphosphate (APP), epoxy resin as a binder with polyamide amine. The stability of the developed coating was verified at 950°C for 1-hour fire test. The results showed that the coating is stable and well bond with the steel substrate. The char was characterized by using FESEM, XRD, FTIR, DTA, TGA, XPS, Py-GCMS and Weathering Test. The morphology of the char was studied by SEM of the coating after furnace fire test. XRD and FTIR show the presence of graphite, borophosphate; boron oxide and sassolite in the residual char. TGA and DTG disclosed that EG improved the residual mass of coating. XPS analysis showed the char residue of IF5-APP-EG contains carbon and oxygen contents 47.50 and 40.70, respectively. Py-GCMS analysis described that the IF5-APP-EG released less gaseous compounds. The weathering test illustrated that's the char expansion of coatings samples was decreased due to the presence of a humid environment and UV light. The IF5-APP-EG showed the maximum char expansion, lower substrate temperature and high residual weight among the studied formulations.