Comparison of Physical,Thermal, and Thermomechanical Properties of Cotton/Epoxy Composite and Cotton/Vinyl Ester Composite Inhibitors

The inhibition of a double‐base solid propellant is used to control and prevent the burning degree of the exposed area, which is due to longer burning time. In recent years, inhibition with cellulose derivatives has become popular, but these monolithic systems usually suffer from the drawback of a high erosion rate and demand high thickness and low burning time. In this research two composite inhibitors based on natural fibers were manufactured by filament winding technique and their physical, thermal, and thermomechanical properties were compared. In addition, a chlorinated flame retardant (CFR) as well as antimony trioxide were added in inhibitor compositions to control their burning processes. It was found that the cotton/epoxy composite inhibitor displays a compatible thermal expansion coefficient with the propellant and a high amount of residual char compared to cotton/vinyl ester composite. Also, it was understood that the moisture absorption resistance and thermal stability, i.e., initial decomposition temperature of cotton/vinyl ester specimen were better than cotton/epoxy specimen. Furthermore, density and the flame retardant performance of both composite inhibitors were similar. Additionally, the tan(δ) value obtained for cotton/epoxy composite was higher than that of cotton/vinyl ester composite indicating its good dissipation of vibrational energy.     

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 phosphorus and sulfur‐containing aromatic diamine curing agent and its application in flame retarded epoxy resins

A novel curing agent of epoxy resins (EPO), bis(3‐amino‐2‐thienyl) phenylphosphine oxide (ABTPPO), was synthesized and characterized by Fourier transform infrared spectroscopy, ¹H nuclear magnetic resonance (NMR), ¹³C NMR, and ³¹P NMR. ABTPPO was used as a flame retardant curing agent, and a novel halogen‐free flame retardant EPO composite was prepared. The flame retardant properties of ABTPPO‐cured EPO were evaluated in terms of limiting oxygen index and vertical burning test (UL‐94), while the combustion and thermal degradation behaviors were investigated by cone calorimeter test (CONE) and thermogravimetric analysis, respectively. The cured EPO composite passed the UL‐94 V‐1 and V‐2 rating when the sample thickness is 3.0 and 1.6 mm, respectively, and the limiting oxygen index value reached 38.3%. The morphological structures of char residue tested by scanning electron microscopy demonstrated that ABTPPO benefited to the formation of a more compact and homogeneous char layer on the materials' surface during burning, which protected the underlying matrix from decomposition and enhanced the flame retardancy of materials. The cured EPO showed excellent fire performance after the water resistance test because of the low water uptake (0.6 wt%), which demonstrated that the flame retardant EPO composite possessed excellent water resistance property. Copyright © 2014 John Wiley & Sons, Ltd.     

A facile method for preparation of PGS@ZB‐N and gas‐sol alternating synergistic effect for fire resistance of EVA

Through the simple precipitation of palygorskite (PGS) by zinc borate (ZB) (to make PGS@ZB) and the decoration of PGS@ZB by dodecylamine (N), a novel organic‐inorganic@inorganic hybrid flame retardant of PGS@ZB‐N was prepared and was incorporated with ethylene vinyl acetate copolymer (EVA) to improve its flame retardance. The structure and morphology of PGS@ZB‐N were characterized by Fourier transform infrared (FTIR) spectroscopy, X‐ray diffraction (XRD), and scanning electron microscopy (SEM), and it was confirmed that the PGS@ZB‐N hybrid had been successfully prepared. The flame retardancy and burning behavior of EVA/PGS@ZB‐N/EG (EG = expandable graphite) composite were studied through thermogravimetric analysis (TGA), limiting oxygen index (LOI), UL‐94 (by the vertical burning test), and cone calorimeter test (CCT) characterizations. The prepared EVA/PGS@ZB‐N/EG composite obtained an LOI value of 41.2% with the addition of 30 wt% PGS@ZB‐N/EG. It was found that EVA/PGS@ZB‐N/EG was protected through a gas phase and condensed phase alternating synergistic effect mechanism.     

Flame retardance and mechanical properties of a polyamide 6/polyethylene/surface‐modified metal hydroxide ternary composite via a master‐batch method

Surface‐modified aluminum hydroxide and magnesium hydroxide mixtures (SAMHs) were filled with linear low‐density polyethylene (LLDPE) with a maleic anhydride grafted polyethylene (PE) compatibilizer to produce a SAMH master batch, which was then dispersed in polyamide 6 (PA6) to yield a PA6/PE/SAMH (50/20/30 by weight ratio) ternary composite. Through such a master‐batch method, an effective flame retardance UL94 V‐0 rating at a 3.2 mm thickness with a 33% limiting oxygen index was achieved. The flame‐retardance mechanism of the ternary composite was investigated by thermogravimetric analysis and scanning electron microscopy/energy dispersive X‐ray spectroscopy analysis. A cocontinuous PA6/PE polymer host and a preferential dispersion of SAMH particles in the matrix induced the formation of a compact flame‐resistant char layer and a high residue rate during burning; this resulted in the desired flame retardance of the ternary composite. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Property of intrinsic flame retardant epoxy resin cured by functional magnesium organic composite salt and diethylenetriamine

An efficient intrinsic flame retardants composite was prepared by curing epoxy resin with a functional magnesium organic composite salt (FMOCS, 0.685 ± 0.3 nm) and diethylenetriamine (DETA). Curing behavior, thermal and flame‐retardant properties of the cured epoxy resins were systematically investigated by infrared spectrum (FTIR), thermogravimetric analysis (TGA), vertical burning test (UL‐94) and limited oxygen index (LOI) measurement. It was found that flame retardancy and mechanical properties of the cured composite are significantly enhanced compared with DETA/EP. The LOI of the EP reached to 33%, which is much higher than the DETA/EP (19%) or its IFR composite (31%) in the optimal addition of ammonium polyphosphate (APP, 18.69 wt %), pentaerythritol (PER, 6.21 wt %) and FMOCS (3.50 wt %). Furthermore, the mechanical properties of the composite material measurement results to imply that it can enhance tensile strength (150%) and bending strength (88%) rather than DETA/EP, which were tested by impact testing machine and microcomputer control electron universal testing machines. Copyright © 2016 John Wiley & Sons, Ltd.     

高分子阻燃剂BPS在PS-HI中的应用研究

通过熔融共混方法将高分子阻燃剂溴代聚苯乙烯 (BPS) 引入高抗冲聚苯乙烯 (PS-HI) 树脂基体中得到两者的共混体系,再在此共混体系中加入适量三氧化二锑 (AO) 和有机化改性蒙脱土 (OMMT) 作为阻燃协效剂,分别用水平燃烧、垂直燃烧、氧指数和高温热分解实验研究了共混体系的阻燃性能。结果表明,BPS本身对PS-HI的阻燃效率较低,加入少量AO就能够使PS-HI/BPS共混体系的阻燃性能显著提高。当PS-HI/BPS/AO的组成为100/30/10时,复合材料的氧指数达到28.1 %,水平和垂直燃烧级别分别达到FH-1级和FV-0级。同时加入AO和OMMT后,复合材料在高温下成炭能力明显增强,其阻燃机理由原来的气相阻燃变为气相与凝固相协同阻燃,但是由于材料的无焰燃烧时间过长,其垂直燃烧级别达不到FV-0级。     

Study on the flame retardancy of EVM/magnesium hydroxide composites optimized with a flame retardant containing phosphorus and silicon

A novel phosphorus‐silicon‐containing flame retardant, spirocyclic pentaerythritol bisphosphorate disphosphoryl chloride/9, 10‐dihydro‐9‐oxa‐10‐phosphaphanthrene‐10‐oxide/vinyl methyl dimethoxysilane (SPDV), was synthesized successfully and used for optimizing the flame retardancy of ethylene‐vinyl acetate copolymer (EVM) rubber/magnesium hydroxide (MDH) composites. The microstructure of SPDV was characterized and determined by Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectroscopy. Thermogravimetric analysis (TGA) showed that SPDV had good charring effect in air even at high temperature (800°C). The flame retardancy of the optimized EVM/MDH composites by SPDV was investigated by limiting oxygen index (LOI), cone calorimeter, and UL‐94 vertical burning tests. A higher LOI value (29.4%) and better UL‐94 rating (V‐0) can be achieved for the optimized EVM/MDH composite (EVM‐7) than EVM/MDH composite without SPDV (EVM‐3) with the total loading of additives. The HRR decreased and residual mass increased gradually as the loading of SPDV increased for the optimized EVM/MDH composites. There existed distinct synergistic intumescent flame‐retardant effect between SPDV and MDH in EVM matrix. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

A facile one‐step synthesis of flame‐retardant coatings on cotton fabric via ultrasound irradiation

This article reports a facile one‐step methodology to increase fire resistance properties of cotton fabric. The flame‐retardant coating for cotton fabric was synthesized with methyltriethoxysilane and organophosphates (M102B) through an ultrasound irradiation process. The coating structure and surface morphology of uncoated and coated fabrics were investigated by Fourier transform infrared spectroscopy and scanning electron microscope, respectively. The flame‐retardant properties, bending modulus, air permeability and thermal stability were studied by vertical burning test, cantilever method, air permeability test and thermogravimetric analysis (TGA). As a result, the cotton fabric coated with 29.2% (mass increased) of flame‐retardant coating was able to balance the flame retardant property and wearing comfort of the fabrics. The TGA results showed that the residue char of cotton was greatly enhanced after treatment with the coating, which has a high char forming effect on cellulose during testing. Furthermore, flame‐retardant property of coated fabrics did not change significantly after 10 washing cycles. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45114.     

Simultaneously enhanced fracture toughness and flame‐retardant property of poly(l‐lactic acid) via reactive blending with ammonium polyphosphate and in situ formed polyurethane

The preparation of poly(l ‐lactic acid) (PLLA) with high mechanical and ideal flame‐retardant properties is a great challenge. Herein, a simultaneous toughness and flame‐retardant PLLA composite was successfully fabricated by using a one‐step process which introduces 4,4′‐methylenediphenyl diisocyanate and ammonium polyphosphate (APP) into PLLA/poly(ε‐caprolactone) blends. SEM, Fourier transform infrared spectroscopy and TGA were adopted to confirm that APP participated in the in situ reaction during the melt process. The impact strength was increased to 13.5 kJ m^?2 from 1.0 kJ m^?2 for L8P2A5 composite, indicating the toughening effect of reactive blending. The cone calorimeter test, limiting oxygen index and vertical burning test results indicate that the flame‐retardant properties of the composites are enhanced with increasing APP content. This work provides a method to prepare PLLA with high mechanical properties and enhanced flame retardancy. © 2020 Society of Chemical Industry     

Synergistic effect between silicone‐containing macromolecular charring agent and ammonium polyphosphate in flame retardant polypropylene

A novel silicone‐containing macromolecular charring agent (Si‐MCA) was synthesized via polycondensation, and it was combined with ammonium polyphosphate (APP) to flame retard polypropylene (PP). The results showed that Si‐MCA exhibited a good synergistic effect with APP in flame retardant PP. When the content of APP was 18.7 wt % and Si‐MCA was 6.3 wt %, the limiting oxygen index value of the PP/APP/Si‐MCA composite was 33.5%, and the vertical burning (UL 94) test classed a V‐0 rating. The peak heat release rate, total heat release, average mass loss rate, and total smoke production of the composite were also decreased significantly. Moreover, the PP/APP/Si‐MCA composite showed an outstanding water resistance. After soaking in 70°C water for 168 h, the PP/APP/Si‐MCA composite could still reach a UL 94 V‐0 rating at 20.0 wt % IFR loading, whereas the PP/APP/PER composite failed to pass the UL 94 test even at 25.0 wt % IFR loading. Thermogravimetric analysis, thermogravimetry‐Fourier transform infrared spectrometry, and scanning electron microscopy‐energy dispersive X‐ray spectrometry results revealed that a compact and thermostable intumescent char was formed by APP/Si‐MCA during burning, thus effectively improved the flame retardancy of PP. The possible synergistic mechanism between APP and Si‐MCA was also discussed. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41580.     

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.     

Preparation and flame retardancy of a novel flame‐retardant poly(ethylene‐co‐vinyl acetate)/aluminum hydroxide composites containing phosphorus

A novel flame‐retardant (SPDH) containing phosphorus was synthesized through the reaction of 10‐(2,5‐dihydroxyphenyl)‐9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide and synthesized intermediate product 3,9‐dichloro‐2,4,8,10‐tetraoxa‐3,9‐diphosphaspiro[5.5] undecane‐3,9‐dioxide, which was used for optimizing the flame retardancy of ethylene‐vinyl acetate copolymer (EVM) rubber/aluminum hydroxide (ATH) composites. The microstructure of SPDH was characterized and determined by Fourier transform infrared and nuclear magnetic resonance spectroscopy. Thermogravimetric analysis (TGA) showed that SPDH had good charring effect at high temperature (600°C). The flame retardancy of the optimized EVM/ATH composites by SPDH was investigated by limiting oxygen index (LOI), cone calorimeter, and UL‐94 vertical burning tests. A higher LOI value (29.8%) and better UL‐94 rating (V‐0) can be achieved for the optimized EVM/ATH composite (EVM‐7) than EVM/ATH composite without SPDH (EVM‐3) with the total loading of additives. The heat release rate decreased and residual mass increased gradually as the loading of SPDH increased for the optimized EVM/ATH composites. There existed distinct synergistic flame‐retardant effect between SPDH and ATH in EVM matrix. POLYM. COMPOS., 2011. © 2011 Society of Plastics Engineers     

The burning behaviors of pool fire flames under low pressure

To investigate the influence of low pressure on pool fire behaviors, liquid n‐heptane pool fires with the diameters of 6, 8, and 10 cm were tested in a low‐pressure altitude chamber. The tests were conducted under different static chamber pressures, ranging from 40 to 60 to 80 to 101 kPa. Fuel mass loss and high‐speed flame video were recorded during the whole burning process of each test. The mass burning intensity is determined by the convective and radiative heat feedback to the fuel, and analysis shows that the convective part is the major contributor to fuel evaporation. Video recordings show that flame height increases with the reduction of pressure, as supported by the dimensionless analysis. The flame puffing amplitude increases under low pressure, resulting in a portion of the flame being quenched. A special phenomenon was observed from the flame videos in that flame rotation emerged at the ending burning stage, which was attributed to the Coriolis force effect. Copyright © 2014 John Wiley & Sons, Ltd.     

Preparation of a novel phosphorus‐ and nitrogen‐containing flame retardant and its synergistic effect in the intumescent flame‐retarding polypropylene system

A novel phosphorus‐ and nitrogen‐containing flame retardant (melamine phytate) was synthesized via the reaction between melamine and phytic acid. The chemical structure of melamine phytate (MPA) was confirmed by Fourier transform‐infrared spectra (FT‐IR) and elemental analysis. And the thermal behavior of MPA investigated by thermogravimetric analysis (TGA) demonstrates that MPA possesses a good char‐forming ability at high temperature. Besides, limiting oxygen index (LOI) and vertical burning tests (UL‐94) illustrate that polypropylene/melamine phytate/dipentaerythritol (PP/MPA/DPER) (70/22.5/7.5) can reach the LOI value of 28.5% and achieve V‐0 rating at the flame retardant loading of 30 wt%. Except that, the thermal weight loss of MPA and DPER in PP composites was investigated by TGA in detail. Moreover, the char residue of PP composite after combustion was systematically analyzed by FT‐IR, scanning electron microscope (SEM) and X‐ray photoelectron spectroscopy (XPS), which can further propose and confirm the flame retardant mechanism. POLYM. COMPOS., 36:1606–1619, 2015. © 2014 Society of Plastics Engineers     

Highly flame‐retardant bio‐based polyurethanes using novel reactive polyols

Poor flame retardancy of polyurethanes (PU) is a global issue as it limits their applications particularly in construction, automobile, and household appliances industries. The global challenge of high flammability of PU can be addressed by incorporating flame‐retardant materials. However, additive flame‐retardants are non‐compatible and depreciate the properties of PU. Hence, reactive flame‐retardants (RFR) based on aliphatic (Ali‐1 and Ali‐2) and aromatic (Ar‐1 and Ar‐2) structured bromine compounds were synthesized and used to prepare bio‐based PU using limonene dimercaptan. The aromatic bromine containing foams showed higher close cell content (average 97 and 100%) and compressive strength (230 and 325 kPa) to that of aliphatic bromine containing foams. Similar behavior was observed for a horizontal burning test where with a low concentration of bromine (5 wt %) in the foams for Ar‐1 and Ar‐2 displayed a burning time of 12.5 and 11.8 s while, Ali‐1 and Ali‐2 displayed burning time of 25.7 and 37 s, respectively. Neat foam showed a burning time of 74 s. The percentage weight loss for neat PU foam was 26.5%, while foams containing 5 wt % bromine in Ali‐1, Ali‐2, Ar‐1, and Ar‐2 foams displayed weight loss of 11.3, 14, 7.9, and 14%, respectively. Our results suggest that flame retardant PU foams could be prepared effectively by using RFR materials. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46027.     

HDPE/APP阻燃型复合材料性能的研究

用聚磷酸铵(APP)对高密度聚乙烯(HDPE)进行改性,制备出不同含量的APP阻燃HDPE复合材料.通过微机控制电子万能试验机、水平-垂直燃烧仪与氧指数测定仪、热重分析(TGA)和扫描电镜(SEM)等研究HDPE/APP阻燃型复合材料的性能.结果表明:随APP的含量增加,HDPE/APP阻燃型复合材料的抗拉强度和弯曲模...     

Flame‐retardant and thermal degradation mechanism of low‐density polyethylene modified with aluminum hypophosphite and microencapsulated red phosphorus

Aluminum hypophosphite (AHP), a novel flame retardant, was used to improve the flame retardancy of low‐density polyethylene (LDPE) with microencapsulated red phosphorus (MRP). The synergistic effect between MRP and AHP was investigated by the limiting oxygen index (LOI), vertical burning test (UL‐94), and thermogravimetric analysis. When the contents of MRP and AHP were 10 and 30 phr, the LOI of LDPE/10MRP/30AHP composite was 25.5%, and it passed the UL‐94 V‐0 rating (the number before “MRP” and “AHP” is the loading of MRP and AHP, In LDPE/10MRP/30AHP, the content of the LDPE, MRP and AHP is 100phr, 10phr and 30phr, where phr refers to parts per hundreds of resin). The results of cone calorimetry testing show that the heat release rate of the composites was significantly reduced, and the strength of the char layer improved when the loading of AHP increased. The thermal stability of the LDPE/10MRP/30AHP composite was enhanced. The structure of the char was investigated by Fourier transform infrared spectrometry and scanning electron microscopy/energy‐dispersive spectrometry. The results indicate that AHP promoted the formation of stable char. This research provided a good way to prepare flame‐retardant materials with a halogen‐free flame retardant and contributed to environmental protection. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43225.     

Preparation technique and property evaluation of flame‐retarding/thermal‐insulating/puncture‐resisting PU foam composites

In this study, flame‐retarding property of PU foam was realized by compounding with flame‐retarding nonwovens in order to stop flame burning and spread. Followed with global warming, thermal‐insulating materials are also used inside of building for energy conservation. This article presents preparation technique and property evaluation of PU composite board composed of composite nonwovens and PU foam by integrating foaming process. By optimization of composite nonwoven, effects of foam density and nonwoven composition on flame‐retarding and thermal‐insulating properties were discussed. Puncture resistance property of composite board was also investigated for resisting against sharp‐object impacts. The resultant composite board would be applied as partition materials in future building decoration. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40463.     

Preparation of aluminum hydroxide/aluminum phosphinate flame‐retardant poly(vinyl alcohol) foam through thermal processing

A novel flame‐retardant poly (vinyl alcohol) (PVA) composite foam was prepared successfully through thermal processing, which was filled with high content of flame retardant, based on aluminum hydroxide (ATH) and aluminum phosphinate (AlPi) and using water as plasticizer and blowing agent. The flame‐retardant property and mechanism of the prepared foam matrix were studied by vertical burning test, limiting oxygen index (LOI), cone calorimeter, scanning electronic microscopy (SEM) and X‐ray photoelectron spectroscopy (XPS). The experimental results showed that the PVA/ATH/AlPi (1/1.2/0.05) composite achieved LOI value of 41% and UL94 V‐0 (3.2 mm) rate. The addition of ATH and AlPi into PVA matrix significantly decreased flammability of the composites, because a more compact and continuous char layer of the PVA/ATH/AlPi composite could be formed, due to the involvement of AlPi in the char‐forming reaction. Compared with the pure PVA sample, the peak heat release rate (PHRR) and total heat release (THR) of PVA/ATH/AlPi (1/1.2/0.05) composite were reduced by 76.5% and 58.2%, respectively. Built upon this PVA‐based foam matrix with good flame retardancy, the flame‐retardant PVA‐based foam was successfully prepared through thermal extrusion. In addition, the influence of water content on melt viscosity, foam structure and mechanical strength was also analyzed. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42020.