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 ◽  
...  

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.

2020 ◽  
Vol 32 (10) ◽  
pp. 1169-1180 ◽  
Author(s):  
Lurong Wang ◽  
Baoping Yang ◽  
Yongliang Guo ◽  
Yabin Zhang ◽  
Niannian Wang ◽  
...  

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.


2018 ◽  
Vol 89 (10) ◽  
pp. 2031-2040 ◽  
Author(s):  
Fanglong Zhu ◽  
QQ Feng ◽  
YF Xu ◽  
JF Hu

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.


2021 ◽  
Author(s):  
Prabhakar M.N. ◽  
K Venkata Chalapathi ◽  
Ur Rehman Shah Atta ◽  
Jung-il Song

Abstract In this study, chitosan-based bio-flame retardant additive (referred to as NCS) was prepared by altering the chitosan (CS) chemically with silica (S) via ion interchange reaction and studied the effect on flame retardant, thermal and mechanical properties of vinyl ester/bamboo fiber (VE/BF) composites manufactured by the vacuum assisted resin transfer molding (VARTM) process. Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis used to characterize the NCS. The spectral results revealed a new peak at 1560 cm-1 corresponding to NH3+–-O Si, bring up the interactive bond between CS and S. SEM, and XRD showed the diverse morphology (coarse surface), and significant decrement in the intensity of diffraction patterns respectively support further the formation of NCS. The heat release rate of NCS decreased significantly by 76%, and residual char increased by 47% compared with chitosan. The flame retardant and thermal behavior of NCS-VE/BF composites were examined by UL-94 standards, micro and cone calorimeter and thermogravimetric analysis. The results showed a delay in burning time in UL-94, enhanced LOI % and decrement of peak heat release rate and total heat release rate compared to pure composites by 32, 14, and 18%, respectively. The residual char increased by 47%. The mechanical properties also improved satisfactorily. Overall, the synthesized NCS could be suitable for the fabrication of sustainable flame-retardant natural fiber composite without deterioration of mechanical properties that are suitable for sub-structural parts in engineering applications.


2018 ◽  
Vol 31 (1) ◽  
pp. 86-96 ◽  
Author(s):  
R Vini ◽  
S Thenmozhi ◽  
SC Murugavel

In this study, azomethine polyphosphonates were synthesized by solution polycondensation of phenylphosphonic dichloride with various azomethine diols such as [4-(4-hydroxy phenyl) iminomethyl] phenol, [(4-(4-hydroxy-3-methoxy phenyl) iminomethyl)] phenol and [4-(4-hydroxy-3-ethoxy phenyl) iminomethyl] phenol using triethylamine catalyst at ambient temperature. The structure of the synthesized polymers was confirmed by Fourier transform infrared and 1H-, 13C- and 31P- nuclear magnetic resonance spectroscopic techniques. Thermal properties of the polymers were studied by thermogravimetric analysis (TGA) and differential scanning calorimetry under nitrogen atmosphere. The TGA data showed that the synthesized polyphosphonates produce high char yield at 600°C due to the presence of phosphorous atom in the polymer chain and hence have good flame-retardant properties. One of the synthesized polyphosphonate was blended with commercial diglycidyl ether of bisphenol-A (DGEBA) resin in various weight percentage and cured with commercial curing agent triethylene tetramine (TETA). The polyphosphonates-blended epoxy thermosets have tensile strength in the range of 5–41 MPa and the percentage of elongation at breaks was 4–18. It was found that the incorporation of polyphosphonates into epoxy thermoset decreased the tensile strength from 41 MPa to 5 MPa, whereas the elongation at break value increased with increase in the weight percentage of polyphosphonate. The influence of polyphosphonates on the flame retardancy of blended thermosets was examined by limiting oxygen index (LOI) and vertical burning (UL-94) tests and found that the polymer samples achieved an increased UL-94 rating and the LOI values were in the range of 24–26. Broido and Horowitz–Metzger methods have been used to study the thermal degradation kinetic parameters.


2018 ◽  
Vol 31 (2) ◽  
pp. 186-196 ◽  
Author(s):  
Shuang Yang ◽  
Yefa Hu ◽  
Qiaoxin Zhang

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.


Polymers ◽  
2019 ◽  
Vol 11 (6) ◽  
pp. 1062 ◽  
Author(s):  
Junlei Chen ◽  
Jihui Wang ◽  
Aiqing Ni ◽  
Hongda Chen ◽  
Penglong Shen

In this work, a novel phosphorous–nitrogen based charring agent named poly(1,3-diaminopropane-1,3,5-triazine-o-bicyclic pentaerythritol phosphate) (PDTBP) was synthesized and used to improve the flame retardancy of high-density polyethylene (HDPE) together with ammonium polyphosphate (APP). The results of Fourier transform infrared spectroscopy (FTIR) and 13C solid-state nuclear magnetic resonance (NMR) showed that PDTBP was successfully synthesized. Compared with the traditional intumescent flame retardant (IFR) system contained APP and pentaerythritol (PER), the novel IFR system (APP/PDTBP, weight ratio of 2:1) could significantly promote the flame retardancy, water resistance, and thermal stability of HDPE. The HDPE/APP/PDTBP composites (PE3) could achieve a UL-94 V-0 rating with LOI value of 30.8%, and had a lower migration percentage (2.2%). However, the HDPE/APP/PER composites (PE5) had the highest migration percentage (4.7%), lower LOI value of 23.9%, and could only achieve a UL-94 V-1 rating. Besides, the peak of heat release rate (PHRR), total heat release (THR), and fire hazard value of PE3 were markedly decreased compared to PE5. PE3 had higher tensile strength and flexural strength of 16.27 ± 0.42 MPa and 32.03 ± 0.59 MPa, respectively. Furthermore, the possible flame-retardant mechanism of the APP/PDTBP IFR system indicated that compact and continuous intumescent char layer would be formed during burning, thus inhibiting the degradation of substrate material and improving the thermal stability of HDPE.


2021 ◽  
Vol 2021 ◽  
pp. 1-11
Author(s):  
MinYi Luo ◽  
Jiayou Xu ◽  
Shu Lv ◽  
XueFeng Yuan ◽  
Xiaolan Liang

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.


2020 ◽  
pp. 002199832096353
Author(s):  
Seda Hazer ◽  
Ayse Aytac

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.


Polymers ◽  
2019 ◽  
Vol 11 (11) ◽  
pp. 1760 ◽  
Author(s):  
Peiyuan Shao ◽  
Peng Xu ◽  
Lei Zhang ◽  
Yun Xue ◽  
Xihui Zhao ◽  
...  

With Cu2+ complexes as precursors, nano-cuprous oxide was prepared on a sodium alginate template excluded of Cl− and based on which the calcium alginate/nano-cuprous oxide hybrid materials were prepared by a Ca2+ crosslinking and freeze-drying process. The thermal degradation and combustion behavior of the materials were studied by related characterization techniques using pure calcium alginate as a comparison. The results show that the weight loss rate, heat release rate, peak heat release rate, total heat release rate and specific extinction area of the hybrid materials were remarkably lower than pure calcium alginate, and the flame-retardant performance was significantly improved. The experimental data indicates that nano-cuprous oxide formed a dense protective layer of copper oxide, calcium carbonate and carbon by lowering the initial degradation temperature of the polysaccharide chain during thermal degradation and catalytically dehydrating to char in the combustion process, and thereby can isolate combustible gases, increase carbon residual rates, and notably reduce heat release and smoke evacuation.


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