Preparation and flame retardancy of an intumescent flame-retardant epoxy resin system constructed by multiple flame-retardant compositions containing phosphorus and nitrogen heterocycle

Yang, Shuang; Wang, Jun; Huo, Siqi; Cheng, Liufeng; Wang, Mei

doi:10.1016/j.polymdegradstab.2015.05.019

Cited by 159 publications

(58 citation statements)

References 36 publications

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“…The FTIR spectra of DOPO and BPD were presented in Figure . The disappearance of P―H stretching vibration at 2437 cm −1 in the FTIR spectrum of BPD demonstrated that DOPO had been completely converted . In addition, the characteristic absorption peaks of N―H (3235 cm −1 ), P―Ph (1598 and 1476 cm −1 ), P―O―Ph (1230, 933, and 755 cm −1 ), P═O (1118 cm −1 ) and P―O―C (1043 cm −1 ) were found in the FTIR spectrum of BPD, confirming the successful synthesis of BPD.…”

Section: Resultsmentioning

confidence: 68%

“…As one of the most common thermosetting resins, epoxy resins (EPs) are subjected in many applications as adhesives and matrix resins . Although EPs possess outstanding adhesion, chemical resistance, and mechanical and electrical insulating properties, EPs are highly flammable, which greatly restricts their applications in many fields where good flame retardancy is required .…”

Section: Introductionmentioning

confidence: 99%

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Flame‐retardant performance and mechanism of epoxy thermosets modified with a novel reactive flame retardant containing phosphorus, nitrogen, and sulfur

Huo

Wang

Yang

et al. 2017

Polymers for Advanced Techs

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A novel phosphorus‐containing, nitrogen‐containing, and sulfur‐containing reactive flame retardant (BPD) was successfully synthesized by 1‐pot reaction. The intrinsic flame‐retardant epoxy resins were prepared by blending different content of BPD with diglycidyl ether of bisphenol‐A (DGEBA). Thermal stability, flame‐retardant properties, and combustion behaviors of EP/BPD thermosets were investigated by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), limited oxygen index (LOI) measurement, UL94 vertical burning test, and cone calorimeter test. The flame‐retardant mechanism of BPD was studied by TGA/infrared spectrometry (TGA‐FTIR), pyrolysis‐gas chromatography/mass spectrometry (Py‐GC/MS), morphology, and chemical component analysis of the char residues. The results demonstrated that EP/BPD thermosets not only exhibited outstanding flame retardancy but also kept high glass transition temperature. EP/BPD‐1.0 thermoset achieved LOI value of 39.1% and UL94 V‐0 rating. In comparison to pure epoxy thermoset, the average of heat release rate (av‐HRR), total heat release (THR), and total smoke release (TSR) of EP/BPD‐1.0 thermoset were decreased by 35.8%, 36.5% and 16.5%, respectively. Although the phosphorus content of EP/BPD‐0.75 thermoset was lower than that of EP/DOPO thermoset, EP/BPD‐0.75 thermoset exhibited better flame retardancy than EP/DOPO thermoset. The significant improvement of flame retardancy of EP/BPD thermosets was ascribed to the blocking effect of phosphorus‐rich intumescent char in condensed phase, and the quenching and diluting effects of abundant phosphorus‐containing free radicals and nitrogen/sulfur‐containing inert gases in gaseous phase. There was flame‐retardant synergism between phosphorus, nitrogen, and sulfur of BPD.

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Section: Resultsmentioning

confidence: 68%

Section: Introductionmentioning

confidence: 99%

Flame‐retardant performance and mechanism of epoxy thermosets modified with a novel reactive flame retardant containing phosphorus, nitrogen, and sulfur

Huo

Wang

Yang

et al. 2017

Polymers for Advanced Techs

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“…The addition of 6.3 wt% of DOPO to DGEBA/DDS reached high LOI value of 35%; however, the samples did not pass any rating in UL 94 test. [12], [18], [20], [35] and [36]. The LOI values of flame-retardant composites were increased by 17% and the UL 94 test results improved from a HB to a V-1 classification with around 1 wt% of phosphorus content.…”

Section: Introductionmentioning

confidence: 96%

Impact of halogen-free flame retardant with varied phosphorus chemical surrounding on the properties of diglycidyl ether of bisphenol-A type epoxy resin: synthesis, fire behaviour, flame-retardant mechanism and mechanical properties

et al. 2016

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This work aimed to investigate the effect of two types of phosphorus-containing flame retardants (P-FRs) with different chemical surroundings (phenylphosphonate-based (PO-Ph) and phenylphosphoric-based (PO-OPh)) on the flameretardant efficiency for diglycidyl ester of bisphenol-A type epoxy (EP) resin. The two series of P-FRs which were named as FPx and FPOx (x=1, 2 and 3), respectively, showed reactivity with epoxy group that was examined by differential scanning calorimetric (DSC) and variable temperatures FTIR spectrum (VT-FTIR). A comparative study between the FPx and FPOx (x=1, 2 and 3) contaning flame-retardamt epoxy was carried out via investigating their flammability, thermal stability and mechanical properties. The most significant difference on flame retardancy between them was that FPx (x=1, 2 and 3) endowed EP with V-0 rating in UL 94 test at 5 wt% loading, while FPOx (x=1, 2 and 3) showed no rating at such loading. Importantly, it is found that there was almost 10 times difference in the flame-retardant efficiency for epoxy resin between FPx and FPOx, though they had similar chemically molecular structures. Moreover, TGA-FTIR and TGA-MS coupling techniques (TGA, thermalgravimetric analysis; MS, mass spectroscopy) were employed to study the thermal decomposition of FP1 and FPO1; the impacts of FP1 and FPO1 on the thermal decomposition of EP were studied by TGA-FTIR as well. Furthermore, an online temperature detection experiment was designed to collect the temperatures by thermocouple and infrared thermometers, respectively in the UL 94 test. Based on the above results, the flame-retardant mechanisms of FP1 and FPO1 in EP were discussed. In addition, the impact of P-FRs on mechanical properties of EP was studied by means of tensile test and dynamic mechanical analysis .

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“…9,10‐Dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO) and DOPO derivatives are verified as an efficient phosphorus‐containing flame retardant for epoxy resin because of their promotion of char layer formation and ability to capture free radicals during combustion . In many cases, phosphorus and nitrogen elements were used together to form a phosphorus‐nitrogen‐containing flame retardant; the synergistic effect between phosphorus and nitrogen endows materials with good flame retardancy .…”

Section: Introductionmentioning

confidence: 99%

A novel halogen‐free co‐curing agent with linear multi‐aromatic rigid structure as flame‐retardant modifier in epoxy resin

Chen

Wang

et al. 2017

Polymers for Advanced Techs

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Preparation and flame retardancy of an intumescent flame-retardant epoxy resin system constructed by multiple flame-retardant compositions containing phosphorus and nitrogen heterocycle

Cited by 159 publications

References 36 publications

Flame‐retardant performance and mechanism of epoxy thermosets modified with a novel reactive flame retardant containing phosphorus, nitrogen, and sulfur

Flame‐retardant performance and mechanism of epoxy thermosets modified with a novel reactive flame retardant containing phosphorus, nitrogen, and sulfur

Impact of halogen-free flame retardant with varied phosphorus chemical surrounding on the properties of diglycidyl ether of bisphenol-A type epoxy resin: synthesis, fire behaviour, flame-retardant mechanism and mechanical properties

A novel halogen‐free co‐curing agent with linear multi‐aromatic rigid structure as flame‐retardant modifier in epoxy resin

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