Assessing the performance of intumescent coatings using bench‐scaled cone calorimeter and finite difference simulations

A method was developed to assess the heat insulation performance of intumescent coatings. The method consists of temperature measurements using the bench‐scaled experimental set‐up of a cone calorimeter and finite difference simulation to calculate the effective thermal conductivity dependent on time/temperature. This simulation procedure was also adapted to the small scale test furnace, in which the standard time–temperature curve is applied to a larger sample and thus which provides results relevant for approval. Investigations on temperature and calculated effective thermal conduction were performed on intumescent coatings in both experimental set‐ups using various coating thicknesses. The results correspond to each other as well as showing the limits of transferability between both fire tests. It is shown that bench‐scaled cone calorimeter tests are a valuable tool for assessing and predicting the performance of intumescent coatings in larger tests relevant for approval. The correlation fails for processes at surface temperatures above 750°C, which are not reached in the cone calorimeter, but are attained in the small scale furnace set‐up. Copyright © 2006 John Wiley & Sons, Ltd.     

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.     

Testing fire protective properties of intumescent coatings by in-line temperature measurements on a cone calorimeter

An experimental setup was proposed for evaluating the thermal shielding efficiency of intumescent coatings. In particular, a cone calorimeter as heater source was coupled with a thermocouple as detector of the temperature of steel plates coated with intumescent coatings. According to ENV 13381-4 test procedure, the heating curves of the setup was measured by plate thermocouple and compared with ISO 834 standard curve. Meanwhile, the comparison was also made between temperature profiles of blank steel plates at different heat fluxes and unprotected steel elements under ISO fire. The possible correlation between bench scale and large scale test was hence discussed. Several factors (heat flux, distance to cone heater, coating thickness, sample size, edge effect and heat insulator) were deeply investigated and discussed: significant relationships between these parameters and the thermal protective properties of the intumescent coating were evidenced; furthermore a fully developed intumescent char could be obtained by controlling the aforementioned parameters. As a conclusion, the proposed bench-scale test was found to be comparable to the large scale test only in the early heating stages.     

New fire‐protective intumescent coatings for wood

Polyurethane coatings are highly flammable, and because of their widespread applications on different substrates (wood, steel, and building materials), there is a need to increase their fire‐safety properties. Intumescent additives sharply suppress the flammability properties of polyurethane coatings. Two problems accompany intumescent additives: their high loading percentage and incompatibility with polyurethane coatings. In this research, we succeeded in increasing the compatibility by mixing intumescent additives with a butyl acrylate polymer and in lowering the flame‐retardant additive loading (up to 20%) by incorporating newly modified montmorillonite. The flammability properties of the new intumescent coatings were characterized with a cone calorimeter. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

超薄膨胀型钢结构防火涂料烃类火试验研究

钢结构建筑属于循环结构形式,由于钢材耐火性能差,温度超过600℃,材料强度和刚度都显著降低,因此必须对钢结构建筑进行防火保护。超薄膨胀型钢结构防火涂料逐渐应用到民用建筑钢结构防火保护中,而且GB14907—2002对其耐火性能评价方法有了具体规定,但是对石化烃类火环境下的耐火性能没有提及。本研究依据GB14907—2002的规定,参照UL1709的实验方法,对烃类火下超薄膨胀型钢结构防火涂料的耐火性能进行了测试。根据试验情况主要考察了涂料的发泡倍数,试验结果表明发泡倍数指标可以作为该类涂料的一个参考指标,并且对烃类火下超薄膨胀型防火涂料的施工养护和粘结强度等提出了建议。     

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.     

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     

空心微珠对膨胀型涂料防火性能的影响

以苯丙乳液为成膜物质,聚磷酸铵、三聚氰胺、季戊四醇为膨胀阻燃体系,以空心玻璃微珠为阻燃协效剂制备了几种防火涂料。用锥形量热仪和小室法研究其燃烧和耐火性能。试验结果表明,空心玻璃微珠会显著提高防火涂料的防火性能。     

Evaluation and characterization of ammoniumpolyphosphate–pentaerythritol‐based systems for intumescent coatings

Intumescent coatings are increasingly used as a method of passive fire protection on steel constructions. By forming a carbon network and releasing a blowing agent, the thin intumescent film swells 100‐fold at elevated temperatures. The highly insulating foam effectively prevents the load bearing steel from reaching its critical temperature at which it looses its mechanical properties and collapses. The role of the carbon donor in intumescent coatings has been studied. Comparison in temperature development, foaming ratios, and rheological behavior has been performed between formulations containing pentaerythritol (penta), di–penta, and tri–penta. A simulated fire test, in which the temperature development during intumescence was studied, showed that the formulations containing penta were considerably more efficient in keeping a low temperature throughout the process. A more rapid temperature development was displayed when using di–penta and tri–penta as the carbon donor. Rheometer tests indicate that penta formulations enter the intumescent process at a lower temperature and stays in it for a longer time than di–penta and tri–penta formulations. Furthermore, the crossover temperature and maximum phase angle are shifted towards higher temperatures by replacing penta with di–penta and with tri–penta in the formulations, respectively. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 748–753, 2007     

Engineering model for intumescent coating behavior in a pilot‐scale gas‐fired furnace

In the event of a fire, intumescent fire protective coatings expand and form a thermally insulating char that protects the underlying substrate from heat and subsequent structural failure. The intumescence includes several rate phenomena, which have been investigated and quantified in the literature for several decades. However, various challenges still exist. The most important one concerns mathematical model validation under realistic exposure conditions and/or time scales. Another is the simplification of advanced models to overcome the often‐seen lack of a complete set of input and adjustable model parameters for a given coating, thereby providing models for industrial applications. In this work, these two challenges are addressed. Three experimental series, with an intumescent coating inside a 0.65 m³ gas‐fired furnace, heating up according to so‐called cellulosic fire conditions, were conducted and a very good repeatability was evident. The experiments were run for almost 3 h, reaching a final gas temperature of about 1100°C. Measurements include transient temperature developments inside the expanding char, at the steel substrate, and in the mineral wool insulation placed behind the substrate. A mathematical model, describing the intumescent coating behavior and temperatures in the furnace using a single overall reaction was developed and validated against experimental data. By including a decomposition front movement through the char, a good qualitative agreement was obtained. After further validation against experiments with other coating formulations, it has potential to become a practical engineering tool. © 2016 American Institute of Chemical Engineers AIChE J, 62: 3947–3962, 2016     

Experimental investigation and numerical modelling of the fire performance for epoxy resin carbon fibre composites of variable thicknesses

This paper applies a unique integrated approach to determine the flammability properties of a composite material (epoxy with carbon fibre) and compares its fire behaviour at two different thicknesses (2.1 and 4.2 mm) by performing small scale (thermo‐gravimetric analysis (TGA)/Fourier transform infrared radiation) and meso‐scale tests (cone calorimeter). For small‐scale tests, experiments were conducted in nitrogen using TGA coupled to gas analysis by Fourier transform infrared radiation. These results allow the determination of thermal stability, main degradation temperature and main gaseous emissions released during the thermal degradation. For meso‐scale tests, experiments were carried out using a cone calorimeter with sample dimensions of 100 × 100 mm at five heat fluxes (30, 40, 50, 60 and 70 kW/m²). The results show that the ignition time increases with an increase in the thickness of the material. Relative hazard classification of the fire performance of the current composites has also been compared with other materials using parameters obtained elsewhere. In addition, the effective ignition, thermal and pyrolysis properties obtained from the ignition and mass loss rate experiments for the 4.2‐mm thick samples were used in a numerical model for pyrolysis to predict well ignition times, back‐surface temperatures and mass pyrolysis rates for all heat fluxes as well as for the 2.1‐mm thick samples. Note that the ignition temperature obtained in the cone agrees with the main degradation temperature in the TGA. The flammability properties deduced here can be used to predict the heat release rate for real fire situations using CFD modelling. Copyright © 2016 John Wiley & Sons, Ltd.     

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.     

Experimental study on insulative properties of intumescent coating exposed to standard and nonstandard furnace curves

This paper reports the results of an experimental study on two types of intumescent coating exposed to the ISO834 standard fire and three nonstandard fire curves. The nonstandard fires were all less severe than the standard fire. A total of 72 intumescent coating protected steel specimens were tested. The expanded thickness of intumescent char was measured, and the pore feature was observed. Constant thermal conductivity for each specimen was calculated based on the measured steel plate temperature. Thermogravimetric analysis (TGA) test was carried out, and the results show that more gas is trapped within the coating due to better matching of thermal behaviour between gas evolution and polymer viscosity as the rate of heating increases. The constant effective thermal conductivities for the intumescent coating under the nonstandard fires were 65% (type‐W) and 35% (type‐S) higher than that under the standard fire, which resulted in an overestimation of the coating failure time up to 15 and 11 minutes, respectively. Therefore, it is sometimes insecure to use results from standard fire tests guiding the design of coating thickness for steel elements under nonstandard fire conditions.     

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.     

紫外老化对溶剂型膨胀防火涂料基本性能的影响

膨胀型钢结构防火涂料的耐候性是其应用中需考虑的一个重要因素。本文利用扫描电镜（ SEM）、热重分析仪（ TG）和小型耐火试验炉研究了紫外老化对膨胀型防火涂料的磷含量、表面形貌、热稳定性和防火性能的影响规律,并研究了面漆对其上述性能的影响。研究结果表明：随紫外老化试验的进行,防火涂料的磷含量、热稳定性、高温膨胀成炭性能和耐火隔热性能均出现明显降低;面漆具有较好的保护作用,表面涂刷面漆的防火涂料各项性能变化不大。     

Thermal shielding performances of nano-structured intumescent coatings containing organo-modified layered double hydroxides

Cone calorimetry tests performed at 50 kW/m² heat flux have been exploited for assessing the fire resistant properties of nano-structured intumescent coatings containing modified layered double hydroxides (hydrotalcites, LDHs) and deposited on steel plates. The effects of different types of modified hydrotalcites (i.e. magnesium–aluminum lactate hydrotalcite, magnesium–aluminum gluconate hydrotalcite, magnesium–aluminum hydrotalcite modified with a fatty acid, magnesium–aluminum hydrotalcite modified with rosin) on the thermal shielding performances of the intumescent coatings and their intumescent degree have been thoroughly discussed and compared with the pristine unfilled counterparts.More specifically, the coatings containing organo-modified LDHs showed better thermal shielding performances with respect to the reference intumescent coating; on the contrary, the use of unmodified hydrotalcite in the intumescent formulations was found detrimental. The thermal shielding performances of the coatings filled with modified LDHs were found to be strictly related to the intumescent degree developed during the cone calorimetry tests. In addition, it was possible to compare the thermal shielding performances of the nanofilled coatings by evaluating the temperatures achieved after 2000 s exposure to the 50 kW/m² heat flux of the cone: the thermal shielding performance sequence was LDH-GL > LDH-RS > LDH-LA > LDH-FA > LDH).Finally, the intumescent degree of the modified coatings was found to decrease with increasing the hydrotalcite content, hence lowering their thermal shielding performances.     

Investigation of char strength and expansion properties of an intumescent coating exposed to rapid heating rates

An efficient and space saving method for passive fire protection is the use of intumescent coatings, which swell when exposed to heat, forming an insulating char layer on top of the virgin coating. Although the temperature curves related to so-called cellulosic fires are often referred to as slow heating curves, special cases where the protective char is mechanically damaged and partly removed can cause extremely fast heating of the coating. This situation, for a solvent based intumescent coating, is simulated using direct insertion of free films into a muffle oven. The char formed is evaluated with respect to the mechanical resistance against compression, degree of expansion, and residual mass fraction. Experimental results show that when using this type of shock heating, the mechanical resistance of the char against compression cannot meaningfully be correlated to the expansion factor. In addition, char properties, measured at room temperature, were dependent on the preceding storage conditions (in air or in a desiccator). The char was found to have the highest mechanical strength against compression in the outer crust facing the heat source. For thin (147 μm) free coating films, a tendency to contract in the horizontal plane was observed. The experimental approach is relevant for testing of intumescent coatings used in buildings where moving or falling objects may damage the char during a fire.     

Vitreous fillers in intumescent coatings

The introduction of vitreous fillers in some intumescent coatings compositions proved to be useful both in improvement of thermal insulation and durability of char under fire and in smoke emission characteristics. In this paper a comprehensive experimental study is presented showing results for solvent-borne, 2K epoxy and water-borne intumescent paints.

Blends of vitreous fillers with different melting temperatures, between 350°C and 850°C, have been tested together with refractory fillers (with melting temperatures between 1100°C and 1350°C). Lead free vitreous fillers with very low melting temperatures (from 350°C to 550°C) and with low water solubility were developed. Different types of paints have been prepared by adding different amounts of vitreous fillers. These compositions were then fire tested after application on steel plates. The effect of vitreous fillers on fire performance and stabilization of char (by means of encapsulation, with or without self-extinguishing additives) has been studied. The fillers’ effect on smoke emission under fire was also examined both in terms of optical density and toxicity index.

A special attention was focused on water-borne intumescent paints modified with vitreous fillers of different solubility and melting temperature. Residual solubility of the vitreous fillers, which appeared as a very important parameter for paint stability, has been assessed. Vitreous fillers releasing alkaline ions in such an amount to give a conductivity higher than 500 μS cm, make the intumescent paint composition unstable.     

新材料在钢结构膨胀型防火涂料中的应用

介绍了改善和提高钢结构膨胀型防火涂料性能的几种新材料，其中晶须材料增加了防火涂料的施工厚度和耐火时间，石墨层间化合物增加了防火涂料的耐火时间和耐水性，氟素改善了防火涂料的理化性能和外观性能，双氢氧化物提高防火涂料的防火性能。     

Laboratory and gas-fired furnace performance tests of epoxy primers for intumescent coatings

Protection of steel structures, using so-called intumescent coatings, is an efficient and space saving way to prolong the time before a building, with load bearing steel constructions, collapses in the event of a fire. In addition to the intumescent coating, application of a primer may be required, either to ensure adhesion of the intumescent coating to the steel or to provide corrosion resistance. It is essential to document the performance of the intumescent coating together with the primer to ensure the overall quality of coating system. In the present work, two epoxy primers were used to investigate the potential failure mechanism of a primer applied prior to an intumescent coating. The analysis was carried out using; (1) gas-fired test furnace, (2) a specially designed electrically heated oven, and (3) thermo gravimetric analysis. When tested below an acrylic intumescent coating, exposed to a gas-fired furnace following the ISO834 fire curve (a so-called cellulosic fire), one of the primers selected performed well and the other poorly. From tests in the electrically heated oven, it was found that both primers were sensitive to the film thickness employed and the presence of oxygen. At oxygen-rich conditions, higher primer thicknesses gave weaker performance. In addition, a color change from red to black was observed in nitrogen, while the color remained red in the oxygen–nitrogen mixture. In summary, the results suggest that an adequate choice of primer, primer thickness, and intumescent coating is essential for a good performance of an intumescent coating system.