Phosphorus-Based α-Amino Acid Mimetic for Enhanced Flame-Retardant Properties in an Epoxy Resin

2019 ◽  
Vol 72 (3) ◽  
pp. 226 ◽  
Author(s):  
Melissa K. Stanfield ◽  
Filip Stojcevski ◽  
Andreas Hendlmeier ◽  
Russell J. Varley ◽  
Jeronimo Carrascal ◽  
...  

This work demonstrates the introduction of a phosphonate moiety into a commonly used curing agent, 4,4′-diaminodiphenylmethane (DDM), via an α-aminophosphonate. This compound (DDMP) can be prepared and isolated in analytical purity in under 1h and in good yield (71%). Thermoset polymer (epoxy-derived) samples were prepared using a room-temperature standard cure (SC) and a post-cured (PC) protocol to encourage incorporation of the α-aminophosphonate into the polymer network, with improved flammability properties observed for the latter. Thermogravimetric analysis under a nitrogen atmosphere showed increased char yield at 600°C, and similar observations were made when analysis was conducted in air. Significant reductions in flammability are observed at very low phosphorus content (P%=0.16–0.49%), demonstrated by higher char yields (25.5 from 14.0% in air), decreased burn time from ignition (60 to 24s), and decreased mass loss after ignition (87.6 to 58.5%). Limiting Oxygen Index for the neat polymer (P%=0%, 20.3±0.8%) increased with increasing α-aminophosphonate additive (P%=0.16%, 20.8±0.6%; P%=0.32%, 21.4±0.4%; P%=0.49%, 22.6±0.8%).

Materials ◽  
2021 ◽  
Vol 14 (12) ◽  
pp. 3230
Author(s):  
Melissa K. Stanfield ◽  
Jeronimo Carrascal ◽  
Luke C. Henderson ◽  
Daniel J. Eyckens

This work demonstrates the introduction of various α-aminophosphonate compounds to an epoxy resin system, thereby improving flame retardance properties. The α-aminophosphonate scaffold allows for covalent incorporation (via the secondary amine) of the compounds into the polymer network. This work explores the synergistic effect of phosphorus and halogens (such as fluorine) to improve flame retardancy. The compounds were all prepared and isolated in analytical purity and in good yield (95%). Epoxy samples were prepared, individually incorporating each compound. Thermogravimetric analysis showed an increased char yield, indicating an improved thermal resistance (with respect to the control sample). Limiting oxygen index for the control polymer was 28.0% ± 0.31% and it increased to 34.6% ± 0.33% for the fluorinated derivative.


2015 ◽  
Vol 30 (6) ◽  
pp. 816-826 ◽  
Author(s):  
Yiren Huang ◽  
Jianwei Yang ◽  
Zhengzhou Wang

Flame-retardant properties of ammonium polyphosphate (APP) and its two microcapsules, APP with a shell of melamine–formaldehyde (MF) resin (MFAPP) and APP with a shell of epoxy resin (EPAPP), were studied in styrene–butadiene–styrene (SBS). The results indicate that APP after the microencapsulation leads to an increase in limiting oxygen index in SBS compared with APP. When dipentaerythritol is incorporated into the SBS composites containing the APP microcapsules, a further improvement in flame retardancy of the composites is observed. The microencapsulation does not result in much improvement of mechanical properties. Moreover, the effect of a compatibilizer (SBS grafted with maleic anhydride) on flame-retardant and mechanical properties of SBS/APP composites was investigated.


Polymers ◽  
2019 ◽  
Vol 11 (10) ◽  
pp. 1708 ◽  
Author(s):  
Wang ◽  
Teng ◽  
Yang ◽  
You ◽  
Zhang ◽  
...  

In this article, the intumescent flame-retardant microsphere (KC-IFR) was prepared by inverse emulsion polymerizations, with the use of k-carrageenan (KC) as carbon source, ammonium polyphosphate (APP) as acid source, and melamine (MEL) as gas source. Meanwhile, benzoic acid functionalized graphene (BFG) was synthetized as a synergist. A “four-source flame-retardant system” (KC-IFR/BFG) was constructed with KC-IFR and BFG. KC-IFR/BFG was blended with waterborne epoxy resin (EP) to prepare flame-retardant coatings. The effects of different ratios of KC-IFR and BFG on the flame-retardant properties of EP were investigated. The results showed that the limiting oxygen index (LOI) values increased from 19.7% for the waterborne epoxy resin to 28.7% for the EP1 with 20 wt% KC-IFR. The addition of BFG further improved the LOI values of the composites. The LOI value reached 29.8% for the EP5 sample with 18 wt% KC-IFR and 2 wt% BFG and meanwhile, UL-94 test reached the V-0 level. In addition, the peak heat release (pHRR) and smoke release rate (SPR) of EP5 decreased by 63.5% and 65.4% comparing with EP0, respectively. This indicated the good flame-retardant and smoke suppression property of EP composites coating.


2012 ◽  
Vol 586 ◽  
pp. 172-176
Author(s):  
Hao Ran Zhou ◽  
Hao Cheng Yang ◽  
An Sun ◽  
Shuang Zhao

As the epoxy potting compound widely used, their flame retardant properties were concerned day by day.This paper neopentyl glycol phosphate melamine salt (NPM) was synthesised via phosphorus oxychloride as the acid source, neopentyl glycol as carbon source, melamine as gas source. The structure of NPM was characterized via infrared spectroscopic analysis (IR). Then the flame retardant properties of NPM/epoxy resin systerm were researched via the limiting oxygen index (LOI), vertical burning experiment, thermal gravimetric analysis (TGA) . The result shows that When the dosage of NPM is 27%, limiting oxygen index of epoxy resin have a extremum, is 32.4, char yield is 18.7% at 600°C. NPM can play a significant role in the improvement of the flame retardant properties of the epoxy.


2018 ◽  
Vol 42 (16) ◽  
pp. 13873-13883 ◽  
Author(s):  
Tianlu Xu ◽  
Chunling Zhang ◽  
Peihong Li ◽  
Xueyan Dai ◽  
Lijie Qu ◽  
...  

Polysiloxane foam (PSF) is a foam material with outstanding performance. However, the limiting oxygen index (LOI) of pure PSF is only 22.0 vol%, which can be attributed to combustible materials.


2016 ◽  
Vol 29 (5) ◽  
pp. 513-523 ◽  
Author(s):  
Tie Zhang ◽  
Weishi Liu ◽  
Meixiao Wang ◽  
Ping Liu ◽  
Yonghong Pan ◽  
...  

With the aim of developing a novel organic flame retardant, an organic boronic acid derivative containing a triazine ring (2,4,6-tris(4-boronic-2-thiophene)-1,3,5-triazine (3TT-3BA)) was synthesized. The thermal properties of 3TT-3BA and its corresponding intermediate products were investigated by thermogravimetric analysis. The results show that 3TT-3BA has a high char yield (56.9%). The flame retardant properties of epoxy resin (EP) with 3TT-3BA were investigated by cone calorimeter, limiting oxygen index (LOI) test, and vertical burning test (UL 94). The LOI of EP with 20% 3TT-3BA is 31.2% and the UL 94 V-0 rating is achieved for EP with 20% 3TT-3BA. The flame retardant mechanism of 3TT-3BA in EP was investigated using TGA–Fourier transform infrared spectroscopy and scanning electron microscopy.


2006 ◽  
Vol 11-12 ◽  
pp. 395-398 ◽  
Author(s):  
Teng Zhang ◽  
Ri Guang Jin

A novel phosphazene cyclomatrix network polymer was synthesized via nucleophilic displacement of activated nitro groups of tri(4-nitrophenoxy)tri(phenoxy) cyclotriphosphazene with the hydroxyls of bisphenol A. Then, thermal properties of the polymer was investigated using dynamic thermogravimetric analysis (TGA) in air, pyrolysis and combustion experiments. According to the relation among the pyrolysis residue (CR) at 850°C, the char-forming tendency (CFT) of every structural unit in polymer and the limiting oxygen index (LOI), CFT of the structural unit (-P=N-)3 and the LOI of the polymer were calculated as 35.04 and 34.3 respectively, which provided theoretical parameter for designing the cyclomatrix- or cyclo- phosphazene polymers with highly thermal and flame-retardant properties.


2015 ◽  
Vol 17 (1) ◽  
pp. 123-133 ◽  
Author(s):  
S. Basak ◽  
Kartick. K. Samanta ◽  
S. Saxena ◽  
S.K. Chattopadhyay ◽  
R. Narkar ◽  
...  

Abstract Flame retardancy was imparted in cellulosic cotton textile using banana pseudostem sap (BPS), an eco-friendly natural product. The extracted sap was made alkaline and applied in pre-mordanted bleached and mercerized cotton fabrics. Flame retardant properties of both the control and the treated fabrics were analysed in terms of limiting oxygen index (LOI), horizontal and vertical flammability. Fabrics treated with the non-diluted BPS were found to have good flame retardant property with LOI of 30 compared to the control fabric with LOI of 18, i.e., an increase of 1.6 times. In the vertical flammability test, the BPS treated fabric showed flame for a few seconds and then, got extinguished. In the horizontal flammability test, the treated fabric showed no flame, but was burning only with an afterglow with a propagation rate of 7.5 mm/min, which was almost 10 times lower than that noted with the control fabric. The thermal degradation and the pyrolysis of the fabric samples were studied using a thermogravimetric analysis (TGA), and the chemical composition by FTIR, SEM and EDX, besides the pure BPS being characterized by EDX and mass spectroscopy. The fabric after the treatment was found to produce stable natural khaki colour, and there was no significant degradation in mechanical strengths. Based on the results, the mechanism of imparting flame retardancy to cellulosic textile and the formation of natural colour on it using the proposed BPS treatment have been postulated.


2015 ◽  
Vol 1115 ◽  
pp. 406-409 ◽  
Author(s):  
Fatimah A’thiyah Sabaruddin ◽  
Noorasikin Samat ◽  
A.I.H Dayang Habibah

It is known that polymeric materials are easily to get on fire due to their chemical structures. Thus the flame retardant material such as aluminium hydroxide (ATH) is used to improve the flame retardancy property of polymers. Polypropylene (PP) with various amount of nanosized ATH particles of (5, 10, 20, 30, 40 wt%) were compounded with an extruder machine. The effects of two different type of coupling agent (3-Aminopropyltriethoxysilane (APS) and Maleic anhydride grafted polypropylene (MAPP)) on the flame retardant properties were compared. All samples were characterized with two flame tests; the limiting oxygen index (LOI) and UL94 horizontal burning test (UL94 HB). It is found that both tests showed improvement on the flame resistance properties of the nanocomposites, mainly at high ATH loadings. Type of coupling agents affects the flame retardancy properties of PP/ATH nanocomposites.


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