Synthesis of multielement phosphazene derivative and the study on flame-retardant properties of epoxy resin

2020 ◽  
Vol 32 (10) ◽  
pp. 1169-1180 ◽  
Author(s):  
Lurong Wang ◽  
Baoping Yang ◽  
Yongliang Guo ◽  
Yabin Zhang ◽  
Niannian Wang ◽  
...  
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Heat Release Rate ◽  
Condensed Phase ◽  
Release Rate ◽  
Photoelectron Spectroscopy ◽  
Carbon Layer ◽  
Limiting Oxygen Index ◽  
Ep Matrix

Herein, we have successfully synthesized phosphorus/nitrogen/silicon tri-elements compound phosphazene derivative hexa-[4-( N-(3-(triethoxysilyl)propyl)acetamide)phenoxy]cyclotriphosphazene (HNTPC) from hexachlorotriphosphazenitrile, methyl 4-hydroxybenzoate, and 3-triethoxysilylpropylamine, and it was used as an additive flame retardant in epoxy resin (EP). Then, the thermal stability and flame retardancy of the composite (HNTPC/EP) were tested. Thermogravimetric analysis showed that the presence of HNTPC made EP matrix decompose at a relatively low temperature, thus promoted the formation of a stable coke layer and protected the matrix from fire. Therefore, the amount of carbon residue was markedly increased at 800°C, indicating an outstanding condensed phase flame-retardant effect. Furthermore, various combustion test data manifested that the addition of HNTPC could significantly improve the flame-retardant performance of EP. In addition, the sample could pass the vertical burning tests (UL-94) V-1 grade when the addition amount was 10% and the limiting oxygen index value was 32.6%, the peak heat release rate and total heat release rate decreased by 40.0% and 21.5%, respectively. Besides, the results of scanning electron microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy also showed that HNTPC can promote the formation of carbon layer and improved the flame-retardant property of EP. Finally, the condensed phase and gas phase synergistic flame-retardant mechanism of HNTPC was proposed.

Synthesis of a phosphorus–nitrogen-containing flame retardant and its application in epoxy resin

2018 ◽  
Vol 31 (2) ◽  
pp. 186-196 ◽  
Author(s):  
Shuang Yang ◽  
Yefa Hu ◽  
Qiaoxin Zhang
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Heat Release Rate ◽  
Flame Retardancy ◽  
Release Rate ◽  
Epoxy Resins ◽  
Proton Nuclear Magnetic Resonance ◽  
Scanning Calorimetry ◽  
Cone Calorimeter Test

In this article, a phosphorus–nitrogen-containing flame retardant (DOPO-T) was successfully synthesized by nucleophilic substitution reaction between 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and cyanuric chloride. The chemical structure of DOPO-T was characterized by Fourier transform infrared spectroscopy, proton nuclear magnetic resonance (NMR) and phosphorous-31 NMR, and elemental analysis. DOPO-T was then blended with diglycidyl ether of bisphenol-A to prepare flame-retardant epoxy resins. Thermal properties, flame retardancy, and combustion behavior of the cured epoxy resins were evaluated by differential scanning calorimetry, thermogravimetric analysis, limited oxygen index (LOI) measurement, UL94 vertical burning test, and cone calorimeter test. The results indicated that the glass transition temperature ( Tg) and temperature at 5% weight loss of epoxy resin (EP)/DOPO-T thermosets were gradually decreased with the increasing content of DOPO-T. DOPO-T catalyzed the decomposition of EP matrix in advance. The flame-retardant performance of EP thermosets was significantly enhanced with the addition of DOPO-T. EP/DOPO-T-0.9 sample had an LOI value of 36.2% and achieved UL94 V-1 rating. In addition, the average of heat release rate, peak of heat release rate, average of effective heat of combustion, and total heat release (THR) of EP/DOPO-T-0.9 sample were decreased by 32%, 48%, 23%, and 31%, respectively, compared with the neat EP sample. Impressively, EP/DOPO-T thermosets acquired excellent flame retardancy under low loading of flame retardant.

scholarly journals Flame-Retardant and Thermal Degradation Mechanism of Caged Phosphate Charring Agent with Melamine Pyrophosphate for Polypropylene

2015 ◽  
Vol 2015 ◽  
pp. 1-11 ◽  
Author(s):  
Xuejun Lai ◽  
Jiedong Qiu ◽  
Hongqiang Li ◽  
Xingrong Zeng ◽  
Shuang Tang ◽  
...  
Keyword(s):  
Thermal Degradation ◽  
Heat Release ◽  
Flame Retardant ◽  
Heat Release Rate ◽  
Release Rate ◽  
Degradation Mechanism ◽  
Limiting Oxygen Index ◽  
Thermal Degradation Mechanism ◽  
Charring Agent ◽  
Ul 94

An efficient caged phosphate charring agent named PEPA was synthesized and combined with melamine pyrophosphate (MPP) to flame-retard polypropylene (PP). The effects of MPP/PEPA on the flame retardancy and thermal degradation of PP were investigated by limiting oxygen index (LOI), vertical burning test (UL-94), cone calorimetric test (CCT), and thermogravimetric analysis (TGA). It was found that PEPA showed an outstanding synergistic effect with MPP in flame retardant PP. When the content of PEPA was 13.3 wt% and MPP was 6.7 wt%, the LOI value of the flame retardant PP was 33.0% and the UL-94 test was classed as a V-0 rating. Meanwhile, the peak heat release rate (PHRR), average heat release rate (AV-HRR), and average mass loss rate (AV-MLR) of the mixture were significantly reduced. The flame-retardant and thermal degradation mechanism of MPP/PEPA was investigated by TGA, Fourier transform infrared spectroscopy (FTIR), TG-FTIR, and scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDXS). It revealed that MPP/PEPA could generate the triazine oligomer and phosphorus-containing compound radicals which changed the thermal degradation behavior of PP. Meanwhile, a compact and thermostable intumescent char was formed and covered on the matrix surface to prevent PP from degrading and burning.

scholarly journals Effects of APP/SiO2polyelectrolyte composites on wood-plastic composite

2019 ◽  
Vol 275 ◽  
pp. 01004
Author(s):  
He Chen ◽  
Shuai Zhang ◽  
Xin Cai ◽  
Mingzhu Pan
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Heat Release Rate ◽  
Release Rate ◽  
Combustion Process ◽  
Cationic Polyelectrolyte ◽  
Carbon Layer ◽  
Limit Oxygen Index ◽  
Crystalline Cellulose ◽  
Plastic Composite

This paper was aimed to evaluate process of APP/SiO2, which used Nano-crystalline cellulose (NCC) modified ammonium polyphosphate (APP) as anionic polyelectrolyte (a-APP), and cationic polyethyleneimine (PEI) modified Nano–SiO2as cationic polyelectrolyte (c-SiO2). The flame retardant system was built due to the reaction of a-APP and c-SiO2. Polyelectrolyte composite of a-APP/c-SiO2were then assembled on the surface of wood powder and HDPE composites. The effect of polyelectrolytes on wood-plastic composites (WPC) were investigated and the results showed that the flame-retardant property of WPC treated by polyelectrolyte was the best. The average heat release rate was 152.8kW/m2, the peak heat release rate was 352.2kW/m2, the total heat release was 108.5kW/m2, the limit oxygen index reached the maximum was 27.5%, compared with the WPC treated by APP, the elongation at break increased by 60.4%. After anionic and cationic polyelectrolyte treatment, making anionized a-APP and cationized c-SiO2due to the charge interaction, in the WPC combustion process to form a dense, uniform WPC carbon layer, thereby reducing the heat transfer to the material inside, and increasing the flame retardancy of WPC composites.

scholarly journals Effects of an Organic-Inorganic Hybrid Containing Allyl Benzoxazine and POSS on Thermal Properties and Flame Retardancy of Epoxy Resin

Polymers ◽  
2019 ◽  
Vol 11 (5) ◽  
pp. 770 ◽  
Author(s):  
Benben Liu ◽  
Huiling Wang ◽  
Xiaoyan Guo ◽  
Rongjie Yang ◽  
Xiangmei Li
Keyword(s):  
Thermal Properties ◽  
Heat Release ◽  
Flame Retardant ◽  
Epoxy Resin ◽  
Heat Release Rate ◽  
Flame Retardancy ◽  
Release Rate ◽  
Cone Calorimeter ◽  
Inorganic Hybrid ◽  
X Ray

A novel organic-inorganic hybrid containing allyl benzoxazine and polyhedral oligomeric silsesquioxane (POSS) was synthesized by the thiol-ene (click) reaction. The benzoxazine (BOZ)-containing POSS (SPOSS-BOZ) copolymerized with benzoxazine/epoxy resin was used to prepare composites of SPOSS-PBZ-E nanocomposites(NPs). The polymerization behavior was monitored by FTIR and non-isothermal differential scanning calorimetry (DSC), which showed that the composites had completely cured with multiple polymerization mechanisms according to the oxazine ring-opening and epoxy resin (EP) polymerization. The thermal properties of the organic–inorganic polybenzoxazine (PBZ) nanocomposites were analyzed by DSC and thermogravimetric analysis (TGA). Furthermore, the X-ray diffraction analysis and the scanning electron microscopy (SEM) micrographs of the SPOSS-PBZ-E nanocomposites indicated that SPOSS was chemically incorporated into the hybrid nanocomposites in the size range of 80–200 nm. The flame retardancy of the benzoxazine epoxy resin composites was investigated by limiting oxygen index (LOI), UL 94 vertical burn test, and cone calorimeter tests. When the amount of SPOSS reached 10% or more, the vertical burning rating of the curing system arrived at V-1, and when the SPOSS-BOZ content reached 20 wt %, the thermal stability and flame retardancy of the material were both improved. Moreover, in the cone calorimeter testing, the addition of SPOSS-BOZ hindered the decomposition of the composites and led to a reduction in the peak heat release rate (pHRR), the average heat release rate (aHRR), and the total heat release (THR) values by about 20%, 25%, and 25%, respectively. The morphologies of the chars were also studied by SEM and energy dispersive X-ray spectroscopy (EDX), and the flame-retardant mechanism of POSS was mainly a condensed-phase flame retardant. The ceramic layer was formed by the enrichment of silicon on the char surface. When there are enough POSS nanoparticles, it can effectively protect the combustion of internal polymers.

scholarly journals Flame Retardancy and Mechanism of Novel Phosphorus-Silicon Flame Retardant Based on Polysilsesquioxane

Polymers ◽  
2019 ◽  
Vol 11 (8) ◽  
pp. 1304 ◽  
Author(s):  
Shengjie Zhu ◽  
Weiguang Gong ◽  
Ji Luo ◽  
Xin Meng ◽  
Zhong Xin ◽  
...  
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Gas Phase ◽  
Condensed Phase ◽  
Flame Retardancy ◽  
Carbon Layer ◽  
Poly Lactic Acid ◽  
Limiting Oxygen Index ◽  
Synergistic Flame Retardant ◽  
Silicon Based

A novel phosphorus-silicon flame retardant (P5PSQ) was prepared by bonding phosphate to silicon-based polysilsesquioxane (PSQ) and used as flame retardant of poly (lactic acid) (PLA). The results show that PLA with 10 wt % P5PSQ has a limiting oxygen index (LOI) 24.1%, the peak heat release rate (PHRR) and total heat release (THR) of PLA decrease 21.8% and 25.2% compared to neat PLA in cone calorimetric test, indicating that P5PSQ shows better flame retardancy in comparison to PSQ. Furthermore, the study for the morphology and composition of carbon residue after the combustion of PLA and the gas release of PLA during combustion illustrate that P5PSQ has flame retardancy in condensed phase and gas phase simultaneously. In condensed phase, phosphorus from phosphate promotes the formation of more stable and better carbon layer containing Si and P, which inhibits the transfer of heat and oxygen in the combustion. In gas phase, the phosphate in P5PSQ emits phosphorus-containing compound that can restrain the release of C–O containing products, which may have effective flame retardancy for PLA in gas phase to a certain extent. In one word, P5PSQ is denoted as a good phosphorus-silicon synergistic flame-retardant.

Intumescent flame retardant coating for polyamide 6,6 (PA 6,6) fabrics containing carbon nanotubes: Synergistic effect of filler on thermal stability and flame retardancy

2018 ◽  
Vol 89 (10) ◽  
pp. 2031-2040 ◽  
Author(s):  
Fanglong Zhu ◽  
QQ Feng ◽  
YF Xu ◽  
JF Hu
Keyword(s):  
Carbon Nanotubes ◽  
Thermal Stability ◽  
Heat Release ◽  
Flame Retardant ◽  
Heat Release Rate ◽  
Flame Retardancy ◽  
Release Rate ◽  
Intumescent Flame Retardant ◽  
Flame Resistance ◽  
Limiting Oxygen Index

Flame retardant mixtures of multi-walled carbon nanotubes (MWCNTs) and intumescent flame retardant (IFR) coatings were applied to polyamide 6,6 (PA 6,6) fabrics to explore whether MWCNTs acted as a good synergist on the thermal stability and flame resistance of the IFR system. The influence of MWCNTs on the flame retardant properties and thermal degradation of the PA 6,6 fabrics were investigated by limiting oxygen index (LOI), vertical burning test (VBT), thermogravimetric analyzer (TGA), scanning electron microscopy (SEM) and cone calorimeter test (CCT). The peak heat release rate and total heat release of the IFR-PA 6,6 fabric with three kinds of wt% MWCNTs were lower than those of the only traditional IFR-PA 6,6 fabric (reduced by 74.2–76.4% and 74.3–76.5%, respectively). As compared to the traditional IFR coating, it was found that no enhancements for thermal stability and flame retardancy in terms of the ability to retard ignition were achieved for the MWCNT/IFR coating. These results demonstrated that the introduction of MWCNTs into an IFR coating can improve the flame retardancy of PA 6,6 fabric in terms of the heat release rate from CCT analysis, but it failed other burning measurements, such as LOI and VBT.

scholarly journals Preparation of Mn2+ Doped Piperazine Phosphate as a Char-Forming Agent for Improving the Fire Safety of Polypropylene/Ammonium Polyphosphate Composites

Materials ◽  
2021 ◽  
Vol 14 (24) ◽  
pp. 7589
Author(s):  
Fuqiang Dong ◽  
Zhonglin Luo ◽  
Biaobing Wang
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Fire Safety ◽  
Raw Materials ◽  
Carbon Layer ◽  
Ammonium Polyphosphate ◽  
Manganese Acetate ◽  
Limiting Oxygen Index ◽  
Peak Heat Release Rate ◽  
High Degree

A piperazine phosphate doped with Mn2+ (HP-Mn), as a new char-forming agent for intumescent flame retardant systems (IFR), was designed and synthesized using 1-hydroxy ethylidene-1,1-diphosphonic acid, piperazine, and manganese acetate tetrahydrate as raw materials. The effect of HP-Mn and ammonium polyphosphate (APP) on the fire safety and thermal stability of polypropylene (PP) was investigated. The results showed that the combined incorporation of 25 wt.% APP/HP-Mn at a ratio of 1:1 endowed the flame retardant PP (PP6) composite with the limiting oxygen index (LOI) of 30.7% and UL-94 V-0 rating. In comparison with the pure PP, the peak heat release rate (PHRR), the total heat release (THR), and the smoke production rate (PSPR) of the PP6 were reduced by 74%, 30%, and 70%, respectively. SEM and Raman analysis of the char residues demonstrated that the Mn2+ displayed a catalytic cross-linking charring ability to form a continuous and compact carbon layer with a high degree of graphitization, which can effectively improve the flame retardancy of PP/APP composites. A possible flame-retardant mechanism was proposed to reveal the synergistic effect between APP and HP-Mn.

scholarly journals Enhanced Thermal Insulation and Flame-Retardant Properties of Polyvinyl Alcohol-Based Aerogels Composited with Ammonium Polyphosphate and Chitosan

2021 ◽  
Vol 2021 ◽  
pp. 1-11
Author(s):  
MinYi Luo ◽  
Jiayou Xu ◽  
Shu Lv ◽  
XueFeng Yuan ◽  
Xiaolan Liang
Keyword(s):  
Polyvinyl Alcohol ◽  
Heat Release ◽  
Flame Retardant ◽  
Thermal Insulation ◽  
Heat Release Rate ◽  
Flame Retardancy ◽  
Release Rate ◽  
Ammonium Polyphosphate ◽  
Composite Aerogel ◽  
Composite Aerogels

Polyvinyl alcohol- (PVA-) based aerogels have attracted widespread attention owing to their low cost, eco-friendliness, and low density. However, the applications of PVA-based aerogels are limited by their flammability. In this study, a flame retardant, ammonium polyphosphate (APP), and a biopolymer, chitosan (CS), were added to polyvinyl alcohol (PVA), and the polymer was further crosslinked using boric acid (H3BO3). In the PVA aerogels, the negatively charged APP and positively charged CS formed a polyelectrolyte complex (PEC) through ionic interaction. Cone calorimetry and vertical burning tests (UL-94) indicated that the PVA composite aerogels have excellent flame retardancy; they could decrease the heat release rate, total heat release rate, and carbon dioxide (CO2) generation. Both PVA/H3BO3 and APP-CS in the composite aerogel could be burned to carbon, and the foamed char layer could act together to impart the PVA composite aerogels with good flame retardancy. Further, the decrease in the temperature at the backside of the aerogels with increasing APP-CS content, as determined by the flame-spraying experiment, indicated that the PVA-based aerogels with APP-CS can also serve as thermal insulation materials. This work provides an effective and promising method for the preparation of PVA-based aerogels with good flame retardancy and thermal insulation property for construction materials.

The influence of various/different ratios synthetic fiber mixture on the mechanical, thermal, morphological and flammability properties of poly (lactic acid)/polycarbonate blend

2020 ◽  
pp. 002199832096353
Author(s):  
Seda Hazer ◽  
Ayse Aytac
Keyword(s):  
Lactic Acid ◽  
Heat Release ◽  
Heat Release Rate ◽  
Release Rate ◽  
Control Sample ◽  
Synthetic Fiber ◽  
Poly Lactic Acid ◽  
Gravimetric Analysis ◽  
Scanning Calorimetry ◽  
Limiting Oxygen Index

Poly (Lactic Acid) (PLA)/Polycarbonate (PC) blend has gained much attention as a bio-based polymeric material in various industrial fields. This study aims to improve the properties of PLA/PC blend reinforced with glass fiber (GF) and carbon fiber (CF) mixture to be produced for industrial use. For this purpose, 50PLA/50PC blend was prepared and used as a control sample. Then, 30% by weight CF and 30% GF were added to the matrix separately. To examine the effect of the use of CF and GF together, the composites were prepared as a mixture form of fibers by adding 5-10-15% CF and 5-10-15% GF, respectively, to the control blend in pairs. All composites compounded with the laboratory-scale twin-screw mini extruder and molded by injection molding. The effects of using synthetic fiber mixture were evaluated in terms of the mechanical, thermal and flammability properties. Differential scanning calorimetry (DSC), thermal gravimetric analysis (TGA), tensile test, scanning electron microscopy (SEM), limiting oxygen index (LOI), heat release rate (HRR) test were carried for the characterization of composites. The highest tensile strength values ​​and maximum % crystallinity values were obtained for the 15CF/15GF fiber mixture containing PLA/PC composite as 113.7 MPa and 21.4, respectively. CO yield (COY), HRR, and total heat release rate were reduced significantly by using synthetic fibers and fiber mixture.

scholarly journals The Fabrication and Properties Characterization of Wood-Based Flame Retardant Composites

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Xia He ◽  
Xianjun Li ◽  
Zhu Zhong ◽  
Yongli Yan ◽  
Qunying Mou ◽  
...  
Keyword(s):  
Heat Release ◽  
Flame Retardant ◽  
Heat Release Rate ◽  
Release Rate ◽  
Untreated Wood ◽  
Smoke Suppression ◽  
Zinc Borate ◽  
Fire Intensity ◽  
Flame Retardation ◽  
Nano Zinc

Wood-based flame retardant composites were fabricated based on vacuum-pressure impregnating method after high intensive microwave pretreatment. The effects of ammonium polyphosphate (APP) and modified nano-zinc borate (nZB) addition on flame-retardation and smoke-suppression properties of wood were investigated by cone calorimeter method (CONE) and thermogravimetric analysis (TGA). The results show that the heat release rate (HRR), peak heat release rate (pk-HRR), and total heat release (THR) of APP-treated woods decreased greatly with increasing concentration of APP. However, mean yield of CO (Mean COY) of APP-treated wood was much higher (3.5 times) than that of untreated wood. Compared with wood treated with APP at a concentration of 15%, the total smoke product (TSP), Mean COY, and pk-HRR decreased by 78.4%, 71.43%, and 31.23%, when wood was treated with APP and nZB (both concentrations were at 15%). APP and nZB have synergistic effects of flame-retardation and smoke-suppression. Nano-zinc borate combined with APP would be used in wood-based composites to efficiently retard flame, reduce fire intensity, and decrease noxious (CO)/smoke release.

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