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     

Epoxy resin/phosphorus‐based microcapsules: Their synergistic effect on flame retardation properties of high‐density polyethylene/graphene nanoplatelets composites

Two types of microcapsule flame retardants are prepared by coating ammonium polyphosphate (APP) and aluminum diethylphosphinate (ADP) with epoxy resin (EP) as the shell via in situ polymerization, and blended with high density polyethylene (HDPE)/graphene nanoplatelets (GNPs) composites to obtain flame‐retardant HDPE materials. Fourier transform infrared spectroscopy, scanning electron microscopy (SEM), and water contact angle results confirm the formation of core–shell structures of EP@APP and EP@ADP. The limiting oxygen index (LOI), vertical burning test (UL‐94), cone calorimetry, and Raman spectroscopy are employed to characterize the HDPE/GNPs composites filled with EP@APP and EP@ADP core–shell materials. A UL94 V‐0 level and LOI of 34% is achieved, and the two flame retardants incorporated in the HDPE/GNPs composite at 20 wt % in total play a synergistic effect in the flame retardancy of the composite at a mass ratio of EP@ADP:EP@APP = 2:1. According to the cone‐calorimetric data, the compounding composites present much lower peak heat release rate (300 kW/m²) and total heat release (99.4 MJ/m²) than those of pure HDPE. Raman spectroscopic analysis of the composites after combustion reveals that the degree of graphitization of the residual char can reach 2.31, indicating the remarkable flame retarding property of the composites. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46662.     

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.     

A novel intumescent flame‐retardant system for flame‐retarded LLDPE/EVA composites

A new intumescent flame retardant (IFR) system consisting of ammonium polyphosphate (APP) and charing‐foaming agent (CFA) and a little organic montmorillonite (OMMT) was used in low‐density polyethylene (LLDPE)/ethylene‐vinyl acetate (EVA) composite. According to limiting oxygen index (LOI) value and UL‐94 rating obtained from this work, the reasonable mass ratio of APP to CFA was 3 : 1, and OMMT could obviously enhance the flame retardancy of the composites. Cone calorimeter (CONE) and thermogravimetric analysis (TGA) were applied to evaluate the burning behavior and thermal stability of IFR‐LLDPE/EVA (LLDPE/EVA) composites. The results of cone calorimeter showed that heat release rate peak (HRR‐peak) and smoke production rate peak (SPR‐peak) and time to ignition (TTI) of IFR‐LLDPE/EVA composites decreased clearly compared with the pure blend. TGA data showed that IFR could enhance the thermal stability of the composites at high temperature and effectively increase the char residue. The morphological structures of the composites observed by scanning electron microscopy (SEM) and X‐ray diffraction (XRD) demonstrated that OMMT could well disperse in the composites without exfoliation, and obviously improve the compatibility of components of IFR in LLDPE/EVA blend. The morphological structures of char layer obtained from Cone indicated that OMMT make the char layer structure be more homogenous and more stable. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Preparation and investigation of flame‐retardant epoxy resin modified with a novel halogen‐free flame retardant containing phosphaphenanthrene,triazine‐trione,and organoboron units

In this article, a novel flame retardant (coded as BNP) was successfully synthesized through the addition reaction between triglycidyl isocyanurate, 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide and phenylboronic acid. BNP was blended with diglycidyl ether of bisphenol‐A to prepare flame‐retardant epoxy resin (EP). Thermal properties, flame retardancy, and combustion behavior of the cured EP were studied by thermogravimetric analysis, limited oxygen index (LOI) measurement, UL94 vertical burning test, and cone calorimeter test. The results indicated that the flame retardancy and smoke suppressing properties of EP/BNP thermosets were significantly enhanced. The LOI value of EP/BNP‐3 thermoset was increased to 32.5% and the sample achieved UL94 V‐0 rating. Compared with the neat EP sample, the peak of heat release rate, average of heat release rate, total heat release, and total smoke production of EP/BNP thermosets were decreased by 58.2%–66.9%, 27.1%–37.9%, 25.8%–41.8%, and 21.3%–41.7%, respectively. The char yields of EP/BNP thermosets were increased by 46.8%–88.4%. The BNP decomposed to produce free radicals with quenching effect and enhanced the charring ability of EP matrix. The multifunctional groups of BNP with flame retardant effects in both gaseous and condensed phases were responsible for the excellent flame retardancy of the EP/BNP thermosets. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45291.     

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     

Flame retardant performance of a carbon source containing DOPO derivative in PET and epoxy

The combination of gas‐phase and condensed‐phase action will contribute to high quality flame retardant. A novel 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO)‐based flame retardant (DOPO‐DOPC), which contains carbon source was synthesized in favor of conducting the effect of gas‐phase as well as promoting the char formation in condensed‐phase. The chemical structure of DOPO‐DOPC was characterized by nuclear magnetic resonance (NMR) and Fourier transform infrared spectroscopy (FTIR). DOPO–DOPC was used as an additive in poly(ethylene terephthalate) (PET) and epoxy resin (EP). The flame retardancy of PET/DOPO‐DOPC and EP/DOPO‐DOPC composites were studied by limiting oxygen index (LOI) and UL‐94 test. The results showed that the incorporation of DOPO–DOPC into PET or EP could obviously improve their flame retardancy. The LOI values of modified PET or EP, which contained 10 wt % DOPO‐DOPC reached 42.8 and 31.7%, respectively. The thermogravimetric analysis (TGA) results revealed that DOPO–DOPC enhanced the formation of char residues. The Laser Raman spectroscopy (LRS) was used to investigate the carbon structure of thermal oxidation residues. Because of the combination of the gas phase flame retardant effect of DOPO moiety and the promoting formation of char residues in condensed phase, the PET and EP composites exhibited significant improvement toward flame retardancy. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44639.     

Synthesis of a novel cross‐linked organophosphorus‐nitrogen containing polymer and its application in flame retardant epoxy resins

A novel cross‐linked organophosphorus–nitrogen polymetric flame retardant additive poly(urea tetramethylene phosphonium sulfate) defined as PUTMPS was synthesized by the condensation polymerization between urea and tetrahydroxymethyl phosphonium sulfate. Its chemical structure was well characterized by Fourier transform infrared (FTIR) spectroscopy, ¹³C and ³¹P solid‐state nuclear magnetic resonance. The synthesized PUTMPS and curing agent m‐phenylenediamine were blended into epoxy resins to prepare flame retardant epoxy resin thermosets. The effects of PUTMPS on fire retardancy and thermal degradation behavior of EP/PUTMPS thermosets were investigated by limiting oxygen index (LOI), vertical burning test (UL‐94), cone calorimeter measurement, and thermalgravimetric analysis (TGA) tests. The surface morphologies and chemical compositions of char residues for cured epoxy resins were investigated by scanning electron microscopy and X‐ray photoelectron spectroscopy (XPS), respectively. Water resistant properties of epoxy resin thermosets were evaluated by putting the samples into distilled water at 70°C for 168 h. The results demonstrated that the EP/12 wt% PUTMPS thermosets successfully passed UL‐94 V‐0 flammability rating and the LOI value reached 31.3%. The TGA results indicated that the incorporation of PUTMPS promoted epoxy resin matrix decomposed and char forming ahead of time, which led to a higher char yield and thermal stability for epoxy resin thermosets at high temperature. The morphological structures and analysis of XPS for the char residues of the epoxy resin thermosets shown that PUTMPS benefited to the formation of a sufficient, more compact, and homogeneous char layer with rich flame retardant elements on the materials surface during burning, which prevented the heat transmission and diffusion, limited the production of combustible gases, inhibited the emission of smoke, and then led to the reduction of the heat release rate and smoke produce rate. After water resistance tests, EP/12 wt% PUTMPS thermosets still remained excellent flame retardancy. Copyright © 2015 John Wiley & Sons, Ltd.     

Flame‐retardant properties of acrylonitrile–butadiene–styrene/wood flour composites filled with expandable graphite and ammonium polyphosphate

Expandable graphite (EG) and ammonium polyphosphate (APP) were used to improve the flame retardancy of acrylonitrile–butadiene–styrene based wood–plastic composites (WPCs). A synergistic effect between EG and APP on the flame retardancy of the WPCs was proposed. The results show that the highest limited oxygen index (LOI) of 34.2% and a V‐0 rating were achieved when the ratio of EG to APP 12.5:7.5; this comprised 20 wt % of the total amount. However, LOI values of the samples with EG and APP alone were only 30.5 and 24.5%, respectively. Thermogravimetric analysis indicated that the flame retardants improved the amount of residue. The EG and EG/APP additives greatly decreased the peak heat release rate and suppressed smoke according to cone calorimetry testing. The scanning electron microscopy analysis indicated that the surface of the wormlike char was covered with a granular substance, which may have been the viscous phosphoric acid or poly(phosphoric acid) decomposed from APP. The flame‐retardant additives worsened the mechanical properties of the WPCs. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40281.     

An easy‐to‐obtain silicone‐containing flame retardant and its effects on the combustion of polycarbonate

A novel silicone‐containing flame retardant (HSOBA) synthesized from hydrogen‐containing silicone oil and Bisphenol A via a simple approach has been incorporated into polycarbonate (PC) matrix to study its effects on the flame retardancy. The flame retardancy of PC/HSOBA composites is investigated by limiting oxygen index (LOI), vertical burning tests (UL‐94), and cone calorimeter measurement. The LOI value of the composites is 31.7 and the UL‐94 rating reaches V‐0, when the content of HSOBA is 3 wt %. Cone calorimeter data confirm that the HSOBA acts as an effective additive functioning both as flame retardants and as smoke suppressant. Evolution of the thermal behaviors of the composites tested by TGA, the morphological structures, and the constituent of char residue after LOI tests characterized by scanning electronic microscopy‐energy‐dispersive X‐ray analysis were used to explain the possible flame‐retardant mode. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Synergistic effect of aluminum hydroxide and nanoclay on flame retardancy and mechanical properties of EPDM composites

The composites based on ethylene–propylene–diene monomer rubber (EPDM) with aluminum hydroxide (ATH), nanoclay, vulcanizing agent, and curing accelerator were prepared by conventional mill compounding method. The thermal stability and the flame retardant properties were evaluated by thermogravimetric analysis (TGA), limiting oxygen index (LOI), UL‐94 test, cone calorimeter, and smoke density chamber tests. The results indicated that the substitution of the nanoclay in the EPDM/ATH composites increased the 50% weight loss temperature and the LOI value, and reduced the peak heat release rate (pk‐HRR), the extinction coefficient (Ext Coef), the maximal smoke density (Dm), and the whole smoke at the first 4 min (VOF4) of the test specimens. The synergistic flame retardancy of the nanoclay with ATH in EPDM matrix could imply that the formation of a reinforced char/nanoclay layer during combustion prevents the diffusion of the oxygen and the decomposed organic volatiles in the flame. The mechanical properties of the composites have been increased by replacing more of the nanoclays into the EPDM/ATH blends. The best loading of the nanoclay in EPDM/ATH composites is 3 wt %, which keeps LOI in the enough value, the V‐0 rating in the UL‐94 test, and the improved mechanical properties with better dispersion and exfoliation of the nanoclays shown by transmission electron microscopy (TEM) micrographs. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 130: 2042–2048, 2013     

Synergistic effect between aluminum hypophosphite and a new intumescent flame retardant system in poly(lactic acid)

A hyperbranched charring agent (CT) was synthesized by triglycidyl isocyanurate and diethylenetriamine in water, and a new intumescent flame retardant (IFR) system was formed by ammonium polyphosphate (APP) and CT. The different formula and synergistic system between IFR and aluminum hypophosphite (AHP) have been studied through limit oxygen index (LOI), UL‐94, cone calorimetry test and TGA. It was found that the LOI for poly(lactic acid) (PLA) with 30 APP/CT (4:1) and 20 wt % IFR/AHP (3:1) were 41.2% and 43.5%, respectively, and the both could achieve UL‐94V‐0 rating with no melt dripping. The heat release rate (HRR), maximum HRR value and average mass loss rate of PLA could be dramatically decreased by combination of IFR and AHP while the thermal stability was greatly enhanced. The study of morphology and structure of char illustrated that more intumescent and compact char layer with good intensity was formed during the degradation of IFR/AHP, which resulting to better flame retardancy and anti‐dripping than IFR or AHP alone. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46359.     

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 phospholipidated β‐cyclodextrin and its application for flame‐retardant poly(lactic acid) with ammonium polyphosphate

In this study, phospholipidated β‐cyclodextrin (PCD) was obtained by the condensation between β‐cyclodextrin and phenyl phosphonic acid dichloride, which was characterized by Fourier transform infrared (FTIR) spectra, ¹H‐NMR, and thermogravimetric analysis (TGA). The thermal stability and flame retardancy of the poly(lactic acid) (PLA) blends [PLA–ammonium polyphosphate (APP)–PCD] were measured by TGA coupled to FTIR spectroscopy, vertical burning test (UL‐94), limiting oxygen index (LOI), and cone calorimetry tests. The results show that the mass ratio and loading amount of APP and PCD affected the properties of PLA. When the loading of APP and PCD was 30 wt % and the mass ratio of APP to PCD was 5:1, the highest LOI value of 42.6% (that of neat PLA was 19.7%) and a UL‐94 V0 rating were achieved, and the reduction of the total heat release was greater than 80%. Even when the total amount of APP and PCD was decreased to 20 wt % with the same mass ratio, the flame‐retardant PLA still can achieved a UL‐94 V0 rating. The improved performance was explained by the formation of an intumescent, continuous, contact char layer. Moreover, the reaction between APP and PCD contributed to the improvement of the thermal stability of the char residue. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46054.     

Application of a novel halogen‐free intumescent flame retardant for acrylonitrile‐butadiene‐styrene

A novel intumescent flame retardant (IFR), containing ammonium polyphosphate (APP) and poly(tetramethylene terephthalamide) (PA4T), was prepared to flame‐retard acrylonitrile‐butadiene‐styrene (ABS). The flame retardation of the IFR/ABS composite was characterized by limiting oxygen index (LOI) and UL‐94 test. Thermogravimetric analysis (TGA) and TGA coupled with Fourier transform infrared spectroscopy (TG‐FTIR) were carried out to study the thermal degradation behavior of the composite and look for the mechanism of the flame‐retarded action. The morphology of the char obtained after combustion of the composite was studied by scanning electron microscopy (SEM). It has been found the intumescent flame retardant showed good flame retardancy, with the LOI value of the PA4T/APP/ABS (7.5/22.5/70) system increasing from 18.5 to 30% and passing UL‐94 V‐1 rating. Meanwhile, the TGA and TG‐FTIR work indicated that PA4T could be effective as a carbonization agent and there was some reaction between PA4T and APP, leading to some crosslinked and high temperature stable material formed, which probably effectively promoted the flame retardancy of ABS. Moreover, it was revealed that uniform and compact intumescent char layer was formed after combustion of the intumescent flame‐retarded ABS composite. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Polyamide‐enhanced flame retardancy of ammonium polyphosphate on epoxy resin

An attractive intumescent flame retardant epoxy system was prepared from epoxy resin (diglycidyl ether of bisphenol A), low molecular weight polyamide (cure agent, LWPA), and ammonium polyphosphate (APP). The cured epoxy resin was served as carbonization agent as well as blowing agent itself in the intumescent flame retardant formulation. Flammability and thermal stability of the cured epoxy resins with different contents of APP and LWPA were investigated by limited oxygen index (LOI), UL‐94 test, and thermogravimetric analysis (TGA). The results of LOI and UL‐94 indicate that APP can improve the flame retardancy of LWPA‐cured epoxy resins. Only 5 wt % of APP can increase the LOI value of epoxy resins from 19.6 to 27.1, and improve the UL‐94 ratings, reaching V‐0 rating from no rating when the mass ratio of epoxy resin to LWPA is 100/40. It is much interesting that LOI values of flame retardant cured epoxy resins (FR‐CEP) increase with decreasing LWPA. The results of TGA, FTIR, and X‐ray photoelectron spectroscopy (XPS) indicate that the process of thermal degradation of FR‐CEP consists of two main stages: the first stage is that a phosphorus rich char is formed on the surface of the material under 500°C, and then a compact char yields over 500°C; the second stage is that the char residue layer can give more effective protection for the materials than the char formed at the first stage do. The flame retardant mechanism also has been discussed according to the results of TGA, FTIR, and XPS for FR‐CEP. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Novel flame‐retardant epoxy composites containing aluminium β‐carboxylethylmethylphosphinate

A novel flame‐retardant aluminum β‐carboxylethylmethylphosphinate [Al(CEP)] was synthesizedby a simple process. The effect of Al(CEP) on the curing of epoxy resin (EP) was investigated with differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy. The flame retardancy and thermal properties of Al(CEP)/EP were analyzed by a limiting oxygen index (LOI), vertical burning test (UL‐94), scanning electron microscopy (SEM) with energy‐dispersive X‐ray (EDX), gravimetric analyses, and DSC. Results disclosed that curing of EP is delayed by incorporating Al(CEP). The flexural strength of EP is reduced but the flexural modulus is increased by adding Al(CEP). Adding Al(CEP) depresses the decomposition of EP while leads to a increase in the glass transition temperature (T_g), in char formation and in flame retardancy of EP. EP containing 25 phr Al(CEP) provides LOI of 28.3% and passes UL‐94 V‐0 rating. SEM results show that the sample passing V‐0 rating can form the condensed char whereas porous char is observed from the sample failing in V‐0 rating after combustion. EDX analysis shows that the condensed char presents higher weight ratio of carbon to phosphorus than the porous char, indicating appropriate amount of Al(CEP) is necessary for formation of the stable char. POLYM. ENG. SCI., 55:657–663, 2015. © 2014 Society of Plastics Engineers     

An effective intumescent flame retardancy of LDPE induced by the combination of APP and CNCO‐HA

A char‐forming agent poly(4,6‐dichloro‐N‐hydroxyethyl?1,3,5‐triazin‐2‐amine‐1,6‐diaminohexane) (CNCO‐HA) containing triazine rings was chosen for improving the flame retardant of low density polyethylene (LDPE). The synergistic effect of CNCO‐HA and Ammonium polyphosphate (APP) on the flame retardancy and char‐forming behavior of LDPE were investigated. The limited oxygen index (LOI) and vertical burning test (UL‐94) results indicated the optimal weight ratio of APP to CNCO‐HA was 3:1, and the LOI value of composite reached 31.0% with 30% intumescent flame retardant (IFR) loading. The cone calorimeter test analysis revealed that IFR presented excellent char forming and smoke suppression ability, and resulted in the efficient decrease of combustibility parameters. The thermogravimetric analysis results demonstrated that IFR reduced the thermal degradation rate at main stage of degradation. Scanning electron microscopy observed that IFR promoted to form a compact and continuous intumescent char layer. The Laser Raman spectroscopy spectra showed that larger graphitization degree was formed to enhance the strength of char, and Fourier transform infrared results presented that P‐O‐C and P‐O‐P structures in the residue char were formed to improve shield performance of the char layer to obtain better flame retardant properties of the composite. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43950.     

Effects of ammonium polyphosphate and triphenyl phosphate on the flame retardancy,thermal, and mechanical properties of glass fiber–reinforced PLA/PC composites

The purpose of this study is to increase of the flammability properties of the glass fiber (GF)–reinforced poly (lactic acid)/polycarbonate (PLA/PC) composites. Ammonium polyphosphate (APP) and triphenyl phosphate (TPP) were used as flame retardants that are including the organic phosphor to increase flame retardancy of GF‐reinforced composites. APP, TPP, and APP‐TPP mixture flame retardant including composites were prepared by using extrusion and injection molding methods. The properties of the composites were determined by the tensile test, limiting oxygen index (LOI), differential scanning calorimetry (DSC), and heat release rate (HRR) test. The minimum T_g value was observed for the TPP including PLA/PC composites in DSC analysis. The highest tensile strength was observed in GF‐reinforced PLA/PC composites. In the LOI test, GF including composite was burned with the lowest concentration of oxygen, and burning time was the longest of this composite. However, the shortest burning time was obtained by using the mixture flame retardant system. The flame retardancy properties of GF‐reinforced PLA/PC composite was improved by using mixture flame retardant. When analyzed the results of HRR, time to ignition (TTI), and mass loss rate together, the best value was obtained for the composite including APP.     

Synthesis of a novel phosphonate flame retardant and its application in epoxy resins

A novel phosphonate flame retardant additive bis(2,6‐dimethyphenyl) phenylphosphonate (BDMPP) was synthesized from phenylphosphonic dichloride and 2,6‐dimethyl phenol, and its chemical structure was characterized by Fourier transform infrared (FTIR) spectroscopy, ¹H and ³¹P nuclear magnetic resonance. The prepared BDMPP and curing agent m‐phenylenediamine were blended into epoxy resins (EP) to prepare flame retardant EP thermosets. The effect of BDMPP on fire retardancy and thermal degradation behavior of EP/BDMPP thermosets was investigated by limiting oxygen index (LOI), vertical burning test (UL‐94), cone calorimeter and thermalgravimetric analysis (TGA). The morphologies of char residues of the EP thermosets were investigated by scanning electron microscopy (SEM) and the water resistant properties of thermosets were evaluated by putting the samples into distilled water at 70°C for 168 h. The results demonstrated that the cured EP/14 wt % BDMPP composites with the phosphorus content of 1.11 wt % successfully passed UL‐94 V‐0 flammability rating and the LOI value was as high as 33.8%. The TGA results indicated that the introduction of BDMPP promoted EP matrix decomposed ahead of time compared with that of pure EP and led to a higher char yield at high temperature. The incorporation of BDMPP enhanced the mechanical properties and reduced the moisture absorption of EP thermosets. The morphological structures of char residue revealed that BDMPP benefited to the formation of a more compact and homogeneous char layer on the materials surface during burning, which prevented the heat transmission and diffusion, limit the production of combustible gases and then lead to the reduction of the heat release rate. After water resistance tests, EP/BDMPP thermosets still remained excellent flame retardancy. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42765.