Flame retardancy and water resistance of novel intumescent flame‐retardant oil‐filled styrene–ethylene–butadiene–styrene block copolymer/polypropylene composites

A novel halogen‐free flame‐retardant composite consisting of an intumescent flame retardant (IFR), oil‐filled styrene–ethylene–butadiene–styrene block copolymer (O‐SEBS), and polypropylene (PP) was studied. On the basis of UL‐94 ratings and limiting oxygen index (LOI) data, the IFRs consisted of a charring–foaming agent, ammonium polyphosphate, and SiO₂ showed very effective flame retardancy and good water resistance in the IFR O‐SEBS/PP composite. When the loading of IFR was only 28 wt %, the IFR–O‐SEBS/PP composite could still attain a UL‐94 V‐0 (1.6 mm) rating, and its LOI value remained at 29.8% after a water treatment at 70°C for 168 h. Thermogravimetric analysis data indicated that the IFR effectively enhanced the temperature of the main thermal degradation peak of the IFR–O‐SEBS/PP composites because of the formation of abundant char residue. The flammability parameters of the composites obtained from cone calorimetry testing demonstrated that water treatment almost did not affect the flammability behavior of the composite. The morphological structures of the char residue and fractured surfaces of the composites were not affected by the water treatment. This was attributed to a small quantity of IFR extracted from the composite. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 39575.     

Preparation of a chitosan‐based flame‐retardant synergist and its application in flame‐retardant polypropylene

A novel flame‐retardant synergist, chitosan/urea compound based phosphonic acid melamine salt (HUMCS), was synthesized and characterized by Fourier transform infrared spectroscopy and ³¹P‐NMR. Subsequently, HUMCS was added to a fire‐retardant polypropylene (PP) compound containing an intumescent flame‐retardant (IFR) system to improve its flame‐retardant properties. The PP/IFR/HUMCS composites were characterized by limiting oxygen index (LOI) tests, vertical burning tests (UL‐94 tests), microscale combustion calorimetry tests, and thermogravimetric analysis to study the combustion behavior and thermal stability. The addition of 3 wt % HUMCS increased the LOI from 31.4 to 33.0. The addition of HUMCS at a low additive amount reduced the peak heat‐release rate, total heat release, and heat‐release capacity obviously. Furthermore, scanning electron micrographs of char residues revealed that HUMCS could prevent the IFR–PP composites from forming a dense and compact multicell char, which could effectively protect the substrate material from combusting. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40845.     

Effect of a novel phosphorus‐containing compound on the flame retardancy and thermal degradation of intumescent flame retardant polypropylene

A novel flame retardant, tetra(5,5‐dimethyl‐1,3‐ dioxaphosphorinanyl‐2‐oxy) neopentane (DOPNP), was synthesized successfully, and its structure was characterized by FT‐IR, ¹H NMR, and ³¹P NMR. The thermogravimetric analysis (TGA) results demonstrate that DOPNP showed a good char‐forming ability. Its initial decomposition temperature was 236.4°C based on 1% mass loss, and its char residue was 41.2 wt % at 600°C, and 22.9 wt % at 800°C, respectively. The flame retardancy and thermal degradation behavior of novel intumescent flame‐retardant polypropylene (IFR‐PP) composites containing DOPNP were investigated using limiting oxygen index (LOI), UL‐94 test, TGA, cone calorimeter (CONE) test, and scanning electron microscopy (SEM). The results demonstrate that DOPNP effectively raised LOI value of IFR‐PP. When the loading of IFR was 30 wt %, LOI of IFR‐PP reached 31.3%, and it passed UL‐94 V‐0. TGA results show that DOPNP made the thermal decomposition of IFR‐PP take place in advance; reduced the thermal decomposition rate and raised the residual char amount. CONE results show that DOPNP could effectively decrease the heat release rate peak of IFR‐PP. A continuous and compact char layer observed from the SEM further proved the flame retardance. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011.     

Synergistic effect of metal oxides on the flame retardancy and thermal degradation of novel intumescent flame‐retardant thermoplastic polyurethanes

The synergistic effects of some metal oxides on novel intumescent flame retardant (IFR)–thermoplastic polyurethane (TPU) composites were evaluated by limiting oxygen index (LOI), vertical burning test (UL‐94), thermogravimetric analysis (TGA), cone calorimetry, and scanning electron microscopy. The experimental data indicated that the metal oxides enhanced the LOI value and restricted the dropping of the composites. The IFR–TPU composites passed the UL‐94 V‐0 rating test (1.6 mm) in the presence of magnesium oxide (MgO) and ferric oxide (Fe₂O₃) at 35 wt % IFR loading, whereas only the MgO‐containing IFR–TPU composite reached a UL‐94 V‐0 rating at 30 wt % IFR loading. The TGA results show that the metal oxides had different effects on the process of thermal degradation of the IFR–TPU compositions. MgO easily reacted with polyphosphoric acid generated by the decomposition of ammonium polyphosphate (APP) to produce magnesium phosphate. MgO and Fe₂O₃ showed low flammability and smoke emission due to peak heat release rate, peak smoke production rate, total heat release, and total smoke production (TSP). However, zinc oxide brought an increase in the smoke production rate and TSP values. Among the metal oxides, MgO provided an impressive promotion on the LOI value. The alkaline metal oxide MgO more easily reacted with APP in IFRs. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Synthesis of novel triazine charring agent and its effect in intumescent flame‐retardant polypropylene

A novel charring agent (CNCA‐DA) containing triazine and benzene ring, using cyanuric chloride, aniline, and ethylenediamine as raw materials, was synthesized and characterized. The effects of CNCA‐DA on flame retardancy, thermal degradation, and flammability properties of polypropylene (PP) were investigated by limited oxygen index (LOI), vertical burning test (UL‐94), thermogravimetric analysis (TGA), and cone calorimeter test (CCT). The TGA results showed that CNCA‐DA had a good char forming ability, and a high initial temperature of thermal degradation; the char residue of CNCA‐DA reached 18.5% at 800°C; Ammonium polyphosphate (APP) could improve the char residue of APP/CNCA‐DA system, the char residue reached 31.6% at 800°C. The results from LOI and UL‐94 showed that the intumescent flame retardant (IFR) containing CNCA‐DA and APP was very effective in flame retardancy of PP. When the mass ratio of APP and CNCA‐DA was 2 : 1, and the IFR loading was 30%, the IFR showed the best effect; the LOI value reached 35.6%. It was also found that when the IFR loading was only 20%, the flame retardancy of PP/IFR can still pass V‐0 rating in UL‐94 tests, and its LOI value reached 27.1%. The CCT results demonstrated that IFR could clearly change the decomposition behavior of PP and form a char layer on the surface of the composites, consequently resulting in efficient reduction of the flammability parameters, such as heat release rate (HRR), total heat release (THR), smoke production rate (SPR), total smoke production (TSP), and mass loss (ML). © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Synergistic effect of kaolinite/halloysite on the flammability and thermostability of polypropylene

Kaolinite (Kaol) and halloysite nanotubes (HNT) are both aluminosilicate clays with similar chemical formulation and different microshapes. In this article, nanotubular HNT and nanoplate Kaol together were introduced into polypropylene (PP) containing intumescent flame retardant (IFR). The flammability of the PP composites was characterized by limiting oxygen index (LOI), vertical burning (UL‐94), and cone calorimeter tests (CCT). The results showed that for the composite with 75 wt % PP and 25 wt % IFR, its LOI was 31.0% and it obtained a UL‐94 grade of V‐2. For the composite of 75 wt % PP, 23.5 wt % IFR, and 1.5 wt % (Kaol/HNT = 9/1), its LOI increased to 36.9 and it obtained a UL‐94 grade of V‐0; at the same time, its peak heat release rate value in CCT decreased by 82.2% compared to neat PP. The thermostability analysis indicated that the mixture of Kaol/HNT could improve the thermostability and final char yield. The char residues were comprehensively analyzed by scanning electron microscopy and Fourier transform infrared spectroscopy. The results illustrated that the Kaol/HNT combination was beneficial to forming a crosslinked network and promoting formation of a compact char with higher strength. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46507.     

Percolation and catalysis effect of bamboo‐based active carbon on the thermal and flame retardancy properties of ethylene vinyl‐acetate rubber

The effect of percolation and catalysis of bamboo‐based active carbon (BAC) on the thermal degradation and flame retardancy of ethylene vinyl‐acetate rubber (EVM) composites with intumescent flame retardants (IFR) consisting of ammonium polyphosphate (APP) and dipentaerythritol (DPER) has been investigated. The vulcanization characteristics were analyzed by a moving die rheometer. Thermogravimetric analysis (TGA) and fire behavior tests such as limiting oxygen index (LOI), vertical burning (UL 94), and cone calorimetry were used to evaluate the thermal properties and flame retardancy of EVM composites. Scanning electron microscopy (SEM) was used to study the morphology of residues of EVM composites. The addition of BAC significantly increased the maximum torque (M_H) of EVM composites and EVM matrices. The combination of IFR with BAC can improve the thermal stability of EVM composites. Moreover, BAC can enhance char residue and promote the formation of a network for IFR. The current EVM/37IFR/3BAC composite achieved an LOI of 33.6% and a UL 94 V‐0 rating. The PHRR, total heat release (THR), and total smoke release (TSR) for EVM/IFR/BAC were greatly reduced as compared to EVM/40IFR. Also, the mechanical properties of the EVMIFR/BAC composites increased with increasing BAC contents. The physical percolation effect between BAC and EVM before and after thermal degradation, and the chemical catalysis effect between BAC and IFR during thermal degradation are responsible for the improved flame retardancy of EVM composites. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42414.     

Synthesis of tris(2‐hydroxyethyl) isocyanurate homopolymer and its application in intumescent flame retarded polypropylene

A macromolecular homopolymer (named as Homo‐THEIC) was synthesized through self‐etherification of tris(2‐hydroxyethyl) isocyanurate (THEIC) molecules and used as charring agent. Its chemical structure was characterized by FTIR and ¹³C‐NMR. The charring agent was mixed with ammonium polyphosphate (APP) and applied in flame retarded polypropylene (PP). Results of UL‐94, LOI, and cone calorimeter test showed that the LOI of flame retarded PP can reach 32.8% and UL‐94 V‐0 rating can be achieved at 30 wt % loading. The heat release rate and smoke production rate during the combustion of PP were substantially reduced. TGA results indicated that the synergistic effect between APP and Homo‐THEIC existed and the addition of intumescent flame retardant (IFR) dramatically enhanced the thermal stability of PP. According to the results of TGA, SEM, TG‐FTIR, FTIR, and Raman, the char forming process of IFR can be separated into three stages: the formation of viscous phosphate ester (T _onset?330 °C), the expanding process along with the decomposition of phosphate ester and the release of a large amount of gases (330–480 °C), and the final formation of graphitic‐like char without any expanding feature (480–670 °C). © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134 , 44663.     

Effects of organopalygorskite on intumescent flame‐retarded polypropylene

The effect of organopalygorskite (OPGS) on an intumescent flame retardant (IFR) low‐density polypropylene (PP) has been investigated using the limited oxygen index (LOI), vertical burning test (UL‐94) and thermogravimetric analysis (TGA). The results of the LOI and UL‐94 tests indicate that the addition of OPGS substantially increases the LOI value for PP/IFR at a OPGS to IRF mass ratio of 2/28 with 30 wt% of total flame retardant. In addition, the samples pass the V‐0 rating in the UL‐94 tests. The results indicate that the addition of 2.0 wt% of OPGS simultaneously increases the tensile strength and bending strength of PP/IFR. J. VINYL ADDIT. TECHNOL., 24:281–287, 2018. © 2016 Society of Plastics Engineers     

Flame retardation and thermal degradation of intumescent flame‐retarded polypropylene composites containing spirophosphoryldicyandiamide and ammonium polyphosphate

A novel halogen‐free intumescent flame retardant, spirophosphoryldicyandiamide (SPDC), was synthesized and combined with ammonium polyphosphate (APP) to produce a compound intumescent flame retardant (IFR). This material was used in polypropylene (PP) to obtain IFR‐PP systems whose flammability and thermal behavior were studied by the limiting oxygen index (LOI) test, UL‐94, thermogravimetric analysis, and cone calorimetry. In addition, the mechanical properties of the systems were investigated. The results indicated that the compound intumescent flame retardant showed both excellent flame retardancy and antidripping ability for PP when the two main components of the IFR coexisted in appropriate proportions. The optimum flame retardant formulation was SPDC:APP = 3:1, which gave an LOI value of 38.5 and a UL‐94 V‐0 rating. Moreover, the heat release rate, production of CO, smoke production rate, and mass loss rate of the IFR‐PP with the optimum formulation decreased significantly relative to those of pure PP, according to the cone calorimeter analysis. The char residues from the cone calorimetry experiments were observed by scanning electron microscopy, which showed that a homogeneous and compact intumescent char layer was formed. J. VINYL ADDIT. TECHNOL., 2010. © 2010 Society of Plastics Engineers     

A novel halogen‐free intumescent flame retardant containing phosphorus and nitrogen and its application in polypropylene systems

A novel halogen‐free intumescent flame retardant, pentaerythritol spirobisphosphoryl‐dicyandiamide (SPDC), was synthesized and characterized by FTIR, ¹H NMR, and ³¹P NMR spectra. The new flame retardant was used in polypropylene (PP) to prepare flame‐retardant materials whose flammability and thermal behavior were studied by the limiting oxygen index (LOI) method, thermogravimetric analysis (TGA), and cone calorimetry (CONE). The mechanical properties were also investigated. The results indicated that when the addition of SPDC reached 30 wt%, the material showed both excellent flame retardancy and anti‐dripping abilities for PP. Moreover, the LOI value of the PP‐IFR(30%) was 32.5, and it passed the UL‐94 V‐0 rating test. The CONE results revealed that in PP, SPDC(30%) significantly decreased the peak heat release, total heat release, and smoke relative to their values for pure PP. The morphological structures observed by SEM demonstrated that SPDC could promote the formation of a homogeneous and compact intumescent char layer. The TGA data showed that SPDC could enhance the thermal stability of PP and effectively increase the char residue formation. J. VINYL ADDIT. TECHNOL., 2010. © 2010 Society of Plastics Engineers     

Flammability and mechanical properties of wood flour‐filled polypropylene composites

Polypropylene (PP) composites filled with wood flour (WF) were prepared with a twin‐screw extruder and an injection‐molding machine. Three types of ecologically friendly flame retardants (FRs) based on ammonium polyphosphate were used to improve the FR properties of the composites. The flame retardancy of the PP/WF composites was characterized with thermogravimetric analysis (TGA), vertical burn testing (UL94‐V), and limiting oxygen index (LOI) measurements. The TGA data showed that all three types of FRs could enhance the thermal stability of the PP/WF/FR systems at high temperatures and effectively increase the char residue formation. The FRs could effectively reduce the flammability of the PP/WF/FR composites by achieving V‐0 UL94‐V classification. The increased LOI also showed that the flammability of the PP/WF/FR composites was reduced with the addition of FRs. The mechanical property study revealed that, with the incorporation of FRs, the tensile strength and flexural strength were decreased, but the tensile and flexural moduli were increased in all cases. The presence of maleic anhydride grafted polypropylene (MAPP) resulted in an improvement of the filler–matrix bonding between the WF/intumescent FR and PP, and this consequently enhanced the overall mechanical properties of the composites. Morphological studies carried out with scanning electron microscopy revealed clear evidence that the adhesion at the interfacial region was enhanced with the addition of MAPP to the PP/WF/FR composites. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Synthesis of amino trimethylene phosphonic acid melamine salt and its application in flame‐retarded polypropylene

Amino trimethylene phosphonic acid melamine salt (MATMP) was synthesized and used as acid source and blowing agent in intumescent flame‐retarded polypropylene (PP); its compositions were characterized by Fourier transform infrared spectroscopy and X‐ray powder diffraction. An intumescent flame retardant (IFR) system composed of MATMP, pentaerythritol (PER), and PP was tested by limiting oxygen index (LOI), UL‐94, cone calorimeter tests, and thermogravimetric analysis and compared with an ammonium polyphosphate (APP)/PER system. The results showed that MATMP had better water resistance than APP, the LOI value of PP/MATMP/PER composite can reach 30.3%, and a UL‐94 V‐0 rating can be reached at 25 wt % IFR loading. The amount of residual char of IFR MATMP/PER was 20.3 and 9.5 wt % at 400 and 600 °C, respectively. A thermooxidative degradation route and a possible flame‐retardant mechanism of IFR were proposed according to the analysis of evolved gases and residual chars. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46274.     

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.     

Synergistic flame retardant effect of BiFeO3 in intumescent flame‐retardant polypropylene composites

The BiFeO₃ was used to intumescent flame retardant (IFR) polypropylene (PP) composites as a synergist. The limiting oxygen index (LOI) and UL‐94 tests indicated that there is an optimum synergistic concentration of BiFeO₃ in the PP/IFR composites. Thermogravimetric analysis (TG) results of flame retardant PP showed that the moderate of BiFeO₃ can reduce the decomposition rate of sample at high temperatures. TG of APP/PER/BiFeO₃ showed that BiFeO₃ main affects the third mass loss stage of APP/PER. So the morphology and composition of the char residue of APP/PER/BiFeO₃ composites were characterized by scanning electron microscopy (SEM), X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS), and laser Raman spectroscopy (LRS). An appropriate amount of BiFeO₃ can react with APP/PER forming Bi O P and Fe O P bond, and so more P elements was involved in a crosslinking reaction to form more stable char residue, which can effectively increase the flame retardant properties of PP. POLYM. COMPOS., 38:2771–2778, 2017. © 2015 Society of Plastics Engineers     

Flammability and thermal degradation of intumescent flame‐retardant polypropylene composites

The flammability of polypropylene (PP) composites containing intumescent flame‐retardant additives, i.e., melamine pyrophosphate (MPP) and 1‐oxo‐4‐hydroxymethyl‐2,6,7‐trioxa‐1‐phosphabicyclo[2.2.2]octane (PEPA) was characterized by limiting oxygen index (LOI), UL 94 test, and cone calorimeter. In addition, the thermal degradation of the composites was studied using thermogravimetric analysis (TG) and real‐time Fourier transform infrared (RTFTIR). It has been found that the PP composite only containing MPP (or PEPA) does not show good flame retardancy even at 30% additive level. Compared with the PP/MPP binary composite, the LOI values of the PP/MPP/PEPA ternary composites at the same additive loading are all increased, and UL 94 rating of the ternary composite (PP3) studied is raised to V‐0 rating from no rating (PP/MPP). The cone calorimeter results show that the heat release rate of some ternary composites decreases in comparison with the binary composite. It is noted from the TG data that initial decomposition temperatures of ternary composites are lower than that of the binary composites. The RTFTIR study indicates that the PP/MPP/PEPA composites have higher thermal oxidative stability than the pure PP. POLYM. ENG. SCI., 2010. © 2009 Society of Plastics Engineers     

Synergistic effect of mesoporous silica SBA‐15 on intumescent flame‐retardant polypropylene

Mesoporous silica SBA‐15 synthesized from Pluronic P123 and tetraethoxysilane was used as a synergistic agent on the flame retardancy of polypropylene (PP)/intumescent flame‐retardant (IFR) system. Limiting oxygen index (LOI), UL‐94 rating and thermogravimetric analysis were used to evaluate the synergistic effect of SBA‐15 on PP/IFR system. It showed that PP/IFR system could reach V‐0 with loading of SBA‐15 ranging from 0.5 to 3 wt%, while without SBA‐15 it had no rating at UL‐94 test. The LOI value increased from 25.5 to 32.2 when the loading of SBA‐15 was 1 wt%. The thermal stability of PP/IFR was improved in the presence of SBA‐15 and the amount of the char residue at 600° C was increased from 8.96 to 16.42 wt% when loading of SBA‐15 varied from 0.5 to 5 wt%. Laser Raman spectroscopy (LRS) and scanning electron microscopy were employed to study the morphology of the char residue of PP/IFR system with and without SBA‐15. Copyright © 2010 John Wiley & Sons, Ltd.     

Preparation and study of intumescent flame retardant poly(butylene succinate) using MgAlZnFe‐CO3 layered double hydroxide as a synergistic agent

Intumescent flame retardant consisting of ammonium polyphosphate and melamine, and MgAlZnFe‐CO₃ layered double hydroxides (LDHs) prepared by the constant pH coprecipitation method, were added to poly(butylene succinate) (PBS) via melt blending to obtain novel intumescent flame retardant poly(butylene succinate) (IFR‐PBS) composites. A study on the effect of MgAlZnFe‐CO₃ LDHs on the mechanical, thermal, and flame retardancy properties of IFR‐PBS composites was investigated. It was revealed that IFR‐PBS composites exhibited both excellent flame retardancy and antidripping properties when the content of MgAlZnFe‐CO₃ LDHs was 1% (the total loading of flame retardant was 20%), for a goal of vertical flammability (UL‐94) V‐0 rate and a limiting oxygen index value of 35. The results showed that a suitable amount of MgAlZnFe‐CO₃ LDHs had a noticeable synergistic effect on IFR‐PBS composites. Importantly, tensile strength and flexural strength were improved by the presence of MgAlZnFe‐CO₃ LDHs. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40736.     

Effect of charring agent THEIC on flame retardant properties of polypropylene

Tris(2‐hydroxyethyl) isocyanurate (THEIC) was used as charring agent and combined with ammonium polyphosphate (APP) to form an intumescent flame retardant (IFR) for polypropylene (PP). The flame retardancy and combustion performance of PP/IFR composite was tested by limiting oxygen index (LOI), UL‐94 vertical burning test and cone calorimeter. The results showed that PP/IFR composite had highest LOI of 34.8 and obtained V‐0 rating when 30 wt % IFR was loaded and mass ratio APP/THEIC was 2 : 1. The peak heat release (PHRR) and total heat release (THR) values of PP composite containing FRs were remarkably reduced compared with that of pure PP. However, water resistant test demonstrated the PP/IFR composite had poor flame retardant durability, both the LOI value and UL‐94 V‐rating decreased when PP/IFR composite was soaked in water at 70°C after 36 h. The degradation process and the char morphology of IFR and PP/IFR composite were investigated by TGA and SEM images. The possible reaction path between APP and THEIC in the swollen process was proposed. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41214.     

Thermal degradation behaviors and flame retardancy of epoxy resins with novel silicon‐containing flame retardant

A novel macromolecular silicon‐containing intumescent flame retardants (Si‐IFR) was synthesized, and its structure was a caged bicyclic macromolecule containing phosphorus‐silicon characterized by IR. Epoxy resins (EP) were modified with Si‐IFR to get the flame retardant EP, whose flammability and burning behavior were characterized by UL 94 and limiting oxygen index (LOI). Twenty percentage of weight of Si‐IFR was doped into EP to get 27.5% of LOI and UL 94 V‐0. The degradation behavior of the flame retardant EP was studied by thermogravimetry, differential thermogravimetry, scanning electron microscopy, and X‐ray photoelectron spectroscopy analysis. The experimental results exhibited that when EP/Si‐IFR was heated, the phosphorus‐containing groups firstly decompose to hydrate the char source‐containing groups to form a continuous and protective carbonaceous char, which changed into heat‐resistant swollen char by gaseous products from the nitrogen‐containing groups. Meanwhile, SiO₂ reacts with phosphate to yield silicophosphate, which stabilizes the swollen char. The barrier properties and thermal stability of the swollen char are most effective in resisting the transport of heat and mass to improve the flame retardancy and thermal stability of EP. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013