A highly efficient intumescent polybutylene succinate: Flame retardancy and mechanistic aspects

Xiao, Fei; Fontaine, Gaëlle; Bourbigot, Serge

doi:10.1016/j.polymdegradstab.2022.109830

Cited by 20 publications

(15 citation statements)

References 60 publications

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“…The 31 P DD‐MAS NMR spectra of flame retarded PBS are shown in Figure 7. It should be noted that the spectra of PBS/IFR10% (Figure 7A) at different times have been reported in our previous work 15 . At 370 s, the bands at −27.3 and −30.9 ppm (corresponding to polyphosphate chain, Q 2 ) disappears, meanwhile, two strong peaks appear at −37.3 and −43.3 ppm, probably indicating the presence of two different crystalline aluminum phosphate species.…”

Section: Resultssupporting

confidence: 70%

“…The 13 C CP‐MAS NMR spectra of flame retarded PBS are shown in Figure 5. For PBS/IFR10% at 130 s, peaks at 173.5, 65.6, 28.1, and 25.3 ppm are assigned to characteristic bands of PBS backbone 15,16 . It should be noted that the spectra are similar for all formulations at earlier stage (ignition stage).…”

Section: Resultsmentioning

confidence: 89%

“…Ethylenediamine phosphate (EDAP) was procured from Chemos GmbH (Germany), melamine poly(aluminum phosphate) (Safire™ 200, MPAlP 30 ) was purchased from Caterna‐Floridienne Chemie (France). It should be noted that the intumescent flame retardant system (IFR) used in this work was composed of EDAP and MPAlP with a mass ratio of 7:3 15 . Moreover, melamine borate (Melagard® MB, MB) was supplied by Italmatch Chemicals (Italy), zinc oxide (Zano® 20, ZnO) was purchased from Umicore Materials (Belgium), zinc carbonate (ZnCO 3 ) was provided by MP Biomedicals (Germany).…”

Section: Methodsmentioning

confidence: 99%

“…In our previous works, a series of intumescent PBS systems based on IFR (e.g., ethylenediamine phosphate 15,16 and piperazine pyrophosphate 2 ) and zinc borate were studied. It was observed that zinc borate shows synergistic flame retardant effect with IFR in PBS due to the formation of crack‐free and reinforced intumescent char layer with improved cohesion and stability during combustion 17 .…”

Section: Introductionmentioning

confidence: 99%

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Solid‐state NMR characterization of multi‐component intumescent flame retardant polybutylene succinate formulations

Xiao

Fontaine

et al. 2022

Polymers for Advanced Techs

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In this work, a series of multi‐component intumescent PBS formulations were elaborated by the combination of intumescent flame retardant (IFR) system (consisting of ethylenediamine phosphate and melamine poly(aluminum phosphate), 7:3, wt:wt) and synergists. Three boron/zinc‐containing compounds (i.e., melamine borate, zinc oxide, zinc carbonate) were examined as potential synergists to improve the fire behavior and fire retardancy of PBS. The MLC results showed that the incorporation of all of these compounds enhanced the fire retardancy of PBS to some extent. Among them, zinc oxide exhibited the best fire retardant performances in terms of reduction of the peak heat release rate (pHRR, −61%), fire growth rate index (FIGRA, −19%), maximum average rate of heat emission (MARHE, −55%), and increase of the time to pHRR (+370 s) and to flameout (+650 s) as compared to PBS/IFR10%. Furthermore, the effect of zinc oxide loading on the fire retardancy of PBS was also investigated, the results showed that 2 wt.% loading exhibited the best performances. Solid‐state NMR characterization indicated that the presence of ZnO resulted in the formation of a crack‐free and dense intumescent char layer reinforced by complex aluminum‐zinc‐phosphates glassy species. The intumescent char layer provided a protective physical barrier with improved flexibility and cohesion, which effectively limits the heat and mass transfer between condensed and gas phases and hence, improving the fire retardancy of PBS.

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Section: Resultssupporting

confidence: 70%

Section: Resultsmentioning

confidence: 89%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Solid‐state NMR characterization of multi‐component intumescent flame retardant polybutylene succinate formulations

Xiao

Fontaine

et al. 2022

Polymers for Advanced Techs

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“…Intumescent flame retardants are a class of halogen-free flame retardants. They have been widely applied in the fire retardancy of polymer composites due to their good antidripping behavior and the low toxic gas emission during burning (compared to halogen-containing flame retardants). − In our previous studies, different intumescent systems were used to enhance the fire retardancy of PBS, such as the ammonium polyphosphate system and the ethylenediamine phosphate system. , Inspired by these studies, in this study, piperazine pyrophosphate (PAPP) is selected as an intumescent system to flame retard PBS. As an all-in-one intumescent flame retardant, PAPP has attracted growing interest due to its high thermal decomposition temperature (temperature of 5% mass loss > 300 °C) and good catalytic carbonization performance .…”

Section: Introductionmentioning

confidence: 99%

Improvement of Flame Retardancy and Antidripping Properties of Intumescent Polybutylene Succinate Combining Piperazine Pyrophosphate and Zinc Borate

Xiao

Fontaine

Bourbigot

2022

ACS Appl. Polym. Mater.

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Developing flame-retarded polybutylene succinate (PBS) is a challenging task owing to its high flammability, noncharring, and melt-dripping during burning. In this work, based on the synergistic combination between piperazine pyrophosphate (PAPP) and zinc borate (ZnB), a promising intumescent PBS system was developed as an efficient strategy to impart PBS with improved flame retardancy and antidripping properties. The results showed that PBS/PAPP15%/ZnB5% passed V-0 rating in the UL-94 vertical burning test (3 mm), while only a V-2 rating was achieved for PBS/PAPP20%. Compared to PBS/PAPP20%, the combination of PAPP and zinc borate (ratio of 15:5) led to significant reductions in the peak heat release rate (pHRR, −55%), fire growth rate index (FIGRA, −40%), and maximum average rate of heat emission (MARHE, −47%) evaluated by mass loss cone calorimetry. Meanwhile, the flame retardancy index of PBS/PAPP15%/ZnB5% reached up to 5.18 and the flameout time significantly increased to 1049 s. Fourier transform infrared and solid-state nuclear magnetic resonance analyses were employed to gain insight into the reaction-to-fire mechanism in the condensed phase. The results confirmed the fact that the formation of a crackfree protective intumescent char layer, reinforced by thermally stable inorganic species (boron−zinc phosphates), effectively restricted the heat and fuel transfer between condensed and gas phases, hence resulting in the excellent enhancement in flame retardancy.

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Synthesis and Characterization of a New Copolymer Consisting of Polyamide 1210 and Reactive Phosphorus−Nitrogen Flame‐Retardant

Qin

Zhou

Gong

et al. 2022

Macromol. Rapid Commun.

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The thermal stability and reactivity of organophosphorus flame-retardants play a critical role in synthesizing copolymerized flame-retardant polyamides. Herein, this work successfully synthesizes a flame-retardant CEPPA-DDA salt (CDS) with both good thermal stability and high reactivity by reacting 2-carboxyethyl phenyl phosphonic acid (CEPPA) with 1,12-dodecanediamine (DDA). Flame-retardant polyamide 1210 (FRPA) is further prepared by copolymerizing the CDS, DDA, and sebacic acid (SEA). The test results show that the introduction of CDS can significantly improve the flame-retardant properties of FRPA. Specifically, the flame-retardant polyamide 1210 (FRPA-7) with 7 wt% CDS addition can reach V-0 grade according to UL-94 standard, accompanying limiting oxygen index value of 30.2% and tensile strength of 38.62 MPa. Compared with pure polyamide 1210, the peak heat release rate and total heat release rate of FRPA-7 reduce by 24.11% and 9.40%, respectively. This study provides a simple strategy to prepare flame-retardant polyamides with high flame retardancy and good mechanical properties, which are expected to show great potentials in future industrial applications.

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A highly efficient intumescent polybutylene succinate: Flame retardancy and mechanistic aspects

Cited by 20 publications

References 60 publications

Solid‐state NMR characterization of multi‐component intumescent flame retardant polybutylene succinate formulations

Solid‐state NMR characterization of multi‐component intumescent flame retardant polybutylene succinate formulations

Improvement of Flame Retardancy and Antidripping Properties of Intumescent Polybutylene Succinate Combining Piperazine Pyrophosphate and Zinc Borate

Synthesis and Characterization of a New Copolymer Consisting of Polyamide 1210 and Reactive Phosphorus−Nitrogen Flame‐Retardant

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