Synthesis of a novel phosphorus‐containing dicyclopentadiene novolac hardener and its cured epoxy resin with improved thermal stability and flame retardancy

A novel phosphorus‐containing dicyclopentadiene novolac (DCPD‐DOPO) curing agent for epoxy resins, was prepared from 9,10‐dihydro‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO) and n‐butylated dicyclopentadiene phenolic resin (DCPD‐E). The chemical structure of the obtained DCPD‐DOPO was characterized with FTIR, ¹H NMR and ³¹P NMR, and its molecular weight was determined by gel permeation chromatography. The flame retardancy and thermal properties of diglycidyl ether bisphenol A (DGEBA) epoxy resin cured with DCPD‐DOPO or the mixture of DCPD‐DOPO and bisphenol A‐formaldehyde Novolac resin 720 (NPEH720) were studied by limiting oxygen index (LOI), UL 94 vertical test and cone calorimeter (CCT), and differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), respectively. It is found that the DCPD‐DOPO cured epoxy resin possess a LOI value of 31.6% and achieves the UL 94 V‐0 rating, while its glass transition temperature (T_g) is a bit lower (133 °C). The T_g of epoxy resin cured by the mixture of DCPD‐DOPO and NPEH720 increases to 137 °C or above, and the UL 94 V‐0 rating can still be maintained although the LOI decreases slightly. The CCT test results demonstrated that the peak heat release rate and total heat release of the epoxy resin cured by the mixture of DCPD‐DOPO and NPEH720 decrease significantly compared with the values of the epoxy resin cured by NPEH720. Moreover, the curing reaction kinetics of the epoxy resin cured by DCPD‐DOPO, NPEH720 or their mixture was studied by DSC. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44599.     

Combustion characteristics and synergistic effects of red phosphorus masterbatch with expandable graphite in the flame retardant HDPE/EVA composites

In this work, the flammability behaviors and synergistic effects of red phosphorus masterbatch (RPM) with expandable graphite (EG) in flame‐retardant high‐density polyethylene/ethylene vinyl‐acetate copolymer (HDPE/EVA) composites have been investigated by limiting oxygen index (LOI), UL‐94 test, cone calorimeter test (CCT), thermogravimetric analysis (TGA), Fourier‐transform infrared (FTIR) and scanning electron microscopy (SEM). The data obtained from LOI, UL‐94 test and CCT showed that suitable amount of RPM had synergistic effects with EG in the HDPE/EVA/EG/RPM composites. The addition of RPM greatly increased the LOI values by 3.4%, obtained UL‐94 V‐0 rating, decreased the heat release rates and total heat release, and prolongated the ignition time when 6.7 phr RPM substituted for EG in the HDPE/EVA/EG/RPM composites. The data from TGA and FTIR spectra also indicated the synergistic effects of RPM with EG considerably enhanced the thermal degradation temperatures. The morphological observations after UL‐94, CCT, and SEM images presented positive evidences that the synergistic effects took place for RPM with EG, and the flame‐retardant mechanism has been changed in flame‐retardant HDPE/EVA/EG/RPM composites. The formation of stable and compact charred residues promoted by RPM acted as effective heat barriers and thermal insulations, which improved the flame‐retardant performances and prevented the underlying polymer materials from burning. POLYM. ENG. SCI., 55:2884–2892, 2015. © 2015 Society of Plastics Engineers     

The flame retardant effect of aluminum phosphinate in combination with zinc borate,borophosphate, and nanoclay in polyamide‐6

The effect of zinc borate (ZnB), borophosphate (BPO₄), and organoclay were studied to improve the flame retardancy of polyamide‐6 composites containing organic phosphinates. The flame retardancy of polyamide‐6 composites was investigated using limiting oxygen index (LOI), Underwriters Laboratories (UL‐94) standard, thermogravimetric analysis, Fourier transform infrared spectroscopy, and mass loss calorimeter. The addition of 15 wt% aluminum phosphinate (AlPi) increased the LOI value from 22.5 to 29.5, and V0 rating was obtained from UL‐94 test. The addition of organoclay, ZnB, and borophosphate does not change the predominant gas phase mechanism of AlPi during LOI and UL‐94 tests. The addition of organoclay increased the condensed phase mechanism of AlPi physically by the protective effect of layered silicate, whereas the addition of ZnB increased the condensed phase mechanism of AlPi chemically by the formation of boron aluminum phosphate species deducted from mass loss calorimeter studies. Copyright © 2012 John Wiley & Sons, Ltd.     

Synthesis of a magnesium/aluminum/iron layered double hydroxide and its flammability characteristics in halogen‐free,flame‐retardant ethylene/vinyl acetate copolymer composites

Mg–Al–Fe ternary hydrotalcites were synthesized by a coprecipitation method and characterized with powder X‐ray diffraction, Fourier transform infrared spectroscopy, and thermogravimetric analysis. The flame‐retardant effects of Mg/Al–CO₃ layered double hydroxides (LDHs) and Mg/Al/Fe–CO₃ LDHs in an ethylene/vinyl acetate copolymer (EVA) were studied with the limited oxygen index (LOI), the UL‐94 test, and the cone calorimeter test (CCT), and the thermal degradation behavior of the composites was examined by thermogravimetric analysis. The results showed that the LOI values of the EVA/(Mg/Al/Fe–CO₃ LDH) composites were basically higher than those of the EVA/(Mg/Al–CO₃ LDH) composites at the same additive level. In the UL‐94 test, there was no rating for the EVA/(Mg/Al–CO₃ LDH) composite at the 50% additive level, and a dripping phenomenon occurred. However, the EVA/(Mg/Al/Fe–CO₃ LDH) composites at the same loading level of LDHs containing a suitable amount of Fe³⁺ ion reached the V‐0 rating, the dripping phenomenon disappearing. The CCTs indicated that the heat release rate (HRR) of the EVA composites with Mg/Al/Fe–CO₃ LDHs containing a suitable amount of Fe³⁺ decreased greatly in comparison with that of the composites with Mg/Al–CO₃ LDHs. The introduction of a given amount of Fe³⁺ ion into Mg/Al–CO₃ LDHs resulted in an increase in the LOI, a decrease in the HRR, and the achievement of the UL‐94 V‐0 rating. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Fabrication of Fly Ash‐Based Mesoporous Aluminosilicate Oxides Loaded with Zinc and its Synergistic Fire Resistancy in Polypropylene

A kind of mesoporous aluminosilicate oxides (MAOs) were fabricated from industrial waste, coal fly ash. After loaded with zinc on MAO, the product MAO‐Zn was characterized by Fourier transform infrared spectroscopy, X‐ray diffraction, thermogravimetric analysis, and scanning electron microscopy (SEM). MAO‐Zn was incorporated with intumescent flame retardant (IFR) together and used in polypropylene (PP). Basic characterization including limiting oxygen index (LOI), vertical burning test (UL‐94), and cone calorimeter test (CCT) were finished. The result showed the LOI value of PP was only 17.7 and cannot pass UL‐94 grade; however, 25 wt% IFR in PP help the composite obtained LOI value of 27.6 and passed UL‐94V‐1 grade. Surprisingly, with only 2 wt% MAO‐Zn substitution of IFR, the LOI of PP/IFR composite sharply went up to 37.2 and passed V‐0 grade. CCT results documented that heat, smoke, and fatal gas release were obviously suppressed by IFR/MAO‐Zn combination. By SEM observation and quantitative analysis of TGA results, the contribution of MAO‐Zn was summarized as adsorption of heat/smoke and promotion on charring. It was worth mentioning that the low dose of MAO‐Zn (≤ 3 wt%) did not bring further deterioration on mechanical properties. J. VINYL ADDIT. TECHNOL., 26:135–143, 2020. © 2019 Society of Plastics Engineers     

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     

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.     

Synergistic effects of fumed silica on intumescent flame‐retardant polypropylene

The synergistic effects of fumed silica on the thermal and flame‐retardant properties of intumescent flame retardant (IFR) polypropylene based on the NP phosphorus‐nitrogen compound have been studied by Fourier transfer infrared (FTIR) spectroscopy, cone calorimeter test (CCT), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), limiting oxygen index (LOI), and UL‐94 tests. The LOI and UL‐94 data show that when ≤1 wt % fumed silica substituted for the IFR additive NP can increase 2 to 4% LOI values of the PP blends and keep the V‐0 rating. The data obtained from the CCT tests indicate the heat release rates (HRR) reduce by about 23% for the PP/NP sample with 0.5 wt % fumed silica, whereas the mass loss rates (MLR) and total heat release (THR) values are much lower than those of the PP/NP samples without fume silica. The TGA data demonstrate that a suitable amount of fumed silica can increase the thermal stability and charred residue of the PP/IFR/SiO₂ blends after 500°C. The morphological structures of charred residues observed by SEM give positive evidence that a suitable amount of fumed silica can promote the formation of compact intumescent charred layers and prevent the charred layers from cracking, which effectively protects the underlying polymer from burning. The dynamic FTIR spectra reveal that the synergistic flame‐retardant mechanism of a suitable amount of fumed silica with IFR additive is due to its physical process in the condensed phases. However, a high loading of fumed silica restricts the formation of charred layers with P? O? P and P? O? C complexes formed from burning of polymer materials and destroys the swelling behavior of intumescent charred layers, which deteriorates the flame retardant and thermal properties of the PP/IFR blends. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Flame‐retardant properties and mechanisms of epoxy thermosets modified with two phosphorus‐containing phenolic amines

Two phosphorus‐containing phenolic amines, a 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO)‐based derivative (DAP) by covalently bonding DOPO and imine (SB) obtained from the condensation of p‐phenylenediamine with salicylaldehyde, and its analog (AP) via the addition reaction between diethyl phosphite and SB, were used to prepare flame‐retardant epoxy resins. The burning behaviors and dynamic mechanical properties of epoxy thermosets were studied by limited oxygen index (LOI) measurement, UL‐94 test, and dynamic mechanical analysis. The flame‐retardant mechanisms of modified thermosets were investigated by thermogravimetric analysis, Py‐GC/MS, Fourier transform infrared, SEM, elemental analysis, and laser Raman spectroscopy. The results revealed that epoxy thermoset modified with DAP displayed the blowing‐out effect during UL‐94 test. With the incorporation of 10 wt % DAP, the modified thermoset showed an LOI value of 36.1% and V‐0 rating in UL‐94 test. The flame‐retardant mechanism was ascribed to the quenching and diluting effect in the gas phase and the formation of phosphorus‐rich char layers in the condensed phase. However, the thermoset modified with 10 wt % AP only showed an LOI value of 25.7% and no rating in UL‐94 test, which was possibly ascribed to the mismatching of charring process with gas emission process during combustion. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43953.     

Expanded polystyrene foams containing ammonium polyphosphate and nano-zirconia with improved flame retardancy and mechanical properties

Expanded polystyrene (EPS) foams were flame retarded using ammonium polyphosphate (APP) and nano-zirconia (nano-ZrO₂) by means of phenolic resin as a binder. It is found that the incorporation of a small amount (5 phr) of nano-ZrO₂ into the APP flame-retarded EPS foams leads to 19% increase in flexural strength and 38% increase in compressive strength. Flame-retardant properties of the flame-retarded EPS foams were investigated by limiting oxygen index (LOI), UL-94 and cone calorimetry test (CCT). The LOI of the APP flame-retarded EPS foams in presence of nano-ZrO₂ is above 31%, and the UL 94 V-0 rating can be reached. The CCT test results indicate that the APP flame-retarded EPS foams containing nano-ZrO₂ have lower peak heat release rate, average effective heat of combustion and average specific extinction area. Moreover, thermal decomposition of the flame-retarded EPS foams was investigated by thermogravimetric analysis (TGA) and the TGA results illustrated clearly that the addition of nano-ZrO₂ into the APP flame-retarded EPS foams leads to an increase in the residual char yield. The reason for the increase is possibly because ZrO₂ may react during combustion process with pyrophosphoric acid produced from the thermal decomposition of APP to form zirconium pyrophosphate (ZrP₂O₇) confirmed by XRD studies of the char, which is helpful to improve the formation of the char. The XPS results showed that the ratio of oxidized carbons in the char increases with the presence of nano-ZrO₂.     

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     

Mechanical,thermal properties,and flame retardancy of PC/ultrafine octaphenyl‐POSS composites

Composites of ultrafine polyhedral oligomeric octaphenyl silsesquioxane (OPS) and polycarbonate (PC) were prepared by melt blending. The mechanical and thermal properties of the composites were characterized by tensile and flexural tests, impact test, differential scanning calorimeter (DSC), dynamic mechanical analysis (DMA), and thermal gravimetric analysis (TGA). Rheological properties of these melts were tested by torque rheometer. The flame retardancy of the composites was tested by limiting oxygen index (LOI), the vertical burning (UL‐94), and cone calorimeter test. The char residue was characterized by scanning electron microscope (SEM) and ATR‐FTIR spectrum. Furthermore, the dispersion of OPS particles in the PC matrix was evidenced by SEM. The results indicate that the glass transition temperatures (T_g) and torque of the composites decrease with increasing OPS loading. The onset decomposition temperatures of composites are lower than that of PC. The LOI value and UL‐94 rating of the PC/OPS composites increase with increasing loading of OPS. When OPS loading reaches 6 wt %, the LOI value is 33.8%, UL‐94 (1.6 mm) V‐0 rating is obtained, and peak heat release rate (PHRR) decreases from 570 to 292 kJ m^?2. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

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     

Flame retardancy and thermal and mechanical performance of intercalated,layered double hydroxide composites of polyamide 11, aluminum phosphinate,and sulfamic acid

Sulfamic acid‐intercalated MgAl‐layered double hydroxide (SA‐LDH) was prepared and added with aluminum phosphinate (AlPi) into polyamide 11 (PA11). The results showed that AlPi/SA‐LDH made a positive contribution to both flame retardancy and thermostability, and the effect was demonstrated with the limiting oxygen index (LOI), vertical burning tests (UL‐94), cone calorimetry (CONE), and thermogravimetric analysis (TGA). The char morphologies were observed by SEM, and its chemical composition was investigated by Fourier transform infrared spectroscopy (FTIR). The decomposition mechanism was examined by TGA‐FTIR. The results showed that the LOI of PA11 was only 23.0 and cannot pass any UL‐94 rating. The addition of 20% AlPi increased the LOI to 31.5 and passed the UL‐94 V‐1 rating, and AlPi/SA‐LDH 15%/5% increased the LOI to 32.4 and also passed the UL‐94 V‐1 rating. The CONE results revealed that 20% of either AlPi or AlPi/SA‐LDH brought about a 30% decrease in the peak heat release rate (pHRR). The contribution of SA‐LDH to flame behavior was especially reflected in the postponement of pHRR. SEM showed that the char morphologies became denser after SA‐LDH incorporation. The improvement in thermal stability of the AlPi/SA‐LDH combination was documented by TGA in both N₂ and air atmospheres. The mechanical performance deterioration caused by AlPi was partly improved by SA‐LDH. The storage modulus (E′) below the T_g of AlPi/SA‐LDH 15%/5% was about 300 MPa higher than with 20% AlPi. This was attributed to a compatibility improvement. The interaction forces among PA11, AlPi, and SA‐LDH were probed by X‐ray photoelectron spectrometry. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43370.     

Flame retardancy and mechanical properties of EVA nanocomposites based on magnesium hydroxide nanoparticles/microcapsulated red phosphorus

The flame retardancy and mechanical properties of ethylene vinyl acetate (EVA) polymer nanocomposite based on magnesium hydroxide (MH) nanoparticles with lamellar‐shape morphological structures and synergistic agent microcapsulated red phosphorus (MRP) have been studied by limiting oxygen index (LOI), cone calorimeter test (CCT), UL‐94 test, tensile strength (TS), and elongation at break (EB). Results showed that LOI values of lamellar‐like nanosized MH (50 × 350 nm²) samples were 1–7 vol. % higher than those of the common micrometer grade MH (1–2 μm) in all additive levels. When 1–3 phr MRP substituted for nanosized MH filler, LOI value increased greatly from original 37 to 55, and met the V‐0 rating in the UL‐94 test. The values of TS for MH nanoparticles composites increased from 10.4 to 17.0 MPa as additive loading levels increased from 80 to 150 phr, respectively, while the corresponding values for common micrometer MH composites decreased steadily from 9.7 to 7.1 MPa. Thermogravimetric analysis (TGA) and dynamic Fourier‐transform infrared spectroscopy (FTIR) results revealed two‐step flame‐retardant mechanism. First, MH particles decompose endothermically with the release of 30.1% hydration water in the 320–370°C temperature range. Second, MRP promote the formation of compact charred layers slowly in the condensed phase in the 450–550°C temperature range. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Synergistic flame retardant effects of ammonium polyphosphate in ethylene‐vinyl acetate/layered double hydroxides composites

Mg–Al–Fe ternary layered double hydroxides (LDH) were synthesized based on bayer red mud by calcination‐rehydration method, and characterized using X‐ray diffraction and thermogravimetric analysis (TGA). The synergistic flame retardant effects of ammonium polyphosphate (APP) with LDH in ethylene‐vinyl acetate (EVA) composites were studied using limiting oxygen index (LOI), UL 94 test, cone calorimeter test (CCT), and smoke density test (SDT). The thermal degradation behavior of EVA/LDH/APP composites was examined by thermal gravimetric analysis‐fourier transform infrared spectrometry (TG‐FTIR). The results showed that LOI values decreased by incorporation of APP together with LDH; and, a suitable amount of APP in EVA/LDH composites can apparently improve UL 94 rating. The CCT results indicated that heat release rate (HRR) of the EVA/LDH/APP composites with APP decreased in comparison with that of the EVA/LDH composites. The SDT results showed that APP was helpful to suppress smoke. The TG‐FTIR data showed that the composites with APP had a higher thermal stability than the EVA/LDH composites at high temperature. POLYM. ENG. SCI., 54:766–776, 2014. © 2013 Society of Plastics Engineers     

A phosphorus‐containing inorganic compound as an effective flame retardant for glass‐fiber‐reinforced polyamide 6

A novel inorganic compound, aluminum hypophosphite (AP), was synthesized successfully and applied as a flame retardant to glass‐fiber‐reinforced polyamide 6 (GF–PA6). The thermal stability and burning behaviors of the GF–PA6 samples containing AP (flame‐retardant GF–PA6) were investigated by thermogravimetric analysis, vertical burning testing (with a UL‐94 instrument), limiting oxygen index (LOI) testing, and cone calorimeter testing (CCT). The thermogravimetric data indicated that the addition of AP decreased the onset decomposition temperatures, the maximum mass loss rate (MLR), and the maximum‐rate decomposition temperature of GF–PA6 and increased the residue chars of the samples. Compared with the neat GF–PA6, the AP‐containing GF–PA6 samples had obviously improved flame retardancy: the LOI value increased from 22.5 to 30.1, and the UL‐94 rating went from no rating to V‐0 (1.6 mm) when the AP content increased from 0 to 25 wt % in GF–PA6. The results of CCT reveal that the heat release rate, total heat release, and MLR of the AP‐containing GF–PA6 samples were lower than those of GF–PA6. Furthermore, the higher additive amount of AP affected the mechanical properties of GF–PA6, but they remained acceptable. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Char barrier effect of graphene nanoplatelets on the flame retardancy and thermal stability of high‐density polyethylene flame‐retarded by brominated polystyrene

Graphene nanoplatelets (GNPs) with the char barrier effect were combined with brominated polystyrene (BPS) and antimony trioxide (Sb₂O₃) to improve the flame retardancy and thermal stability of high‐density polyethylene. Thermogravimetric analysis, limited oxygen index (LOI) testing, and vertical burning testing (UL‐94) showed that the presence of GNPs led to enhanced thermal oxidation stability and significantly reduced the flammability. The addition of 1 wt % GNPs to polyethylene/BPS–Sb (mass ratio = 92/6/2) led to UL‐94 grades from NG (first burning time > 30 s) to V‐2 (total burning time = 14 s), and the LOI value increased from 23.4 to 24.1%. The results of the pyrolysis products provided evidence that the GNPs restricted volatilization. The morphology of the chars also proved the formation of the char layer, which could act as a barrier to isolate the material from the flame and retard the vaporization of flammable gases via a tortuous pathway. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40520.     

Synthesis of a novel flame retardant containing phosphorus and sulfur and its application in polycarbonate

A novel flame retardant containing phosphorus and sulfur, bis(2‐tienyl)phenylphosphine (BTPP) was synthesized and characterized with Fourier transform infrared spectroscopy, ¹H, ¹³C, and ³¹P nuclear magnetic resonance. BTPP was used to impart flame retardancy to polycarbonate (PC). Combustion behaviors and thermal degradation properties of PC/BTPP system were assayed by limiting oxygen index (LOI), vertical burning test (UL‐94), cone calorimeter test, and thermogravimetric analysis. PC/3 wt% BTPP passed UL‐94 V‐0 rating with 3.0 mm samples and the LOI value was 36.5%. PC/6 wt% BTPP passed UL‐94 V‐0 rating with 1.6 mm samples and the LOI value was 38.5%. Scanning electron microscopy revealed that char properties had direct effects on the flame retardancy. Mechanical properties and water resistance of PC/BTPP system were also examined. After water resistance test, PC/3 wt% BTPP with 3.0 mm samples and PC/6 wt% BTPP with 1.6 mm samples kept V‐0 rating and mass loss were only 0.2%. POLYM. ENG. SCI., 2012. © 2012 Society of Plastics Engineers     

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.