Synthesis of charring agent and its derivatives of dipentaerythritol polycyclicphosphonates flame retardants

Zhi, Huizhen; Zhou, Hao; Cao, Yang; Yang, Xufeng; Zhang, Weiwei; Jinfei, Yang

doi:10.1080/02533839.2014.953238

Journal of the Chinese Institute of Engineers

2014

DOI: 10.1080/02533839.2014.953238

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Synthesis of charring agent and its derivatives of dipentaerythritol polycyclicphosphonates flame retardants

Huizhen Zhi

Hao Zhou

Yang Cao

et al.

Abstract: Charring agent (dipentaerythritol (DPER) biphosphite) was synthesized and characterized by Fourier transform infrared (FTIR), hydrogen nuclear magnetic resonance, and elemental analysis. Then, three halogen-free intumescent flame retardants, DPER biphosphite trimethyl phosphate (DTMP), DPER biphosphite triethyl phosphate (DTEP), and DPER biphosphite dimethyl methyl phosphonate (DDMMP) were prepared and highly thermally stable polymers were obtained. FTIR demonstrated that new peaks of P-C and P=O were formed i… Show more

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Cited by 4 publications

References 33 publications

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Combining Mechanical Fortification and Ultralow Flammability in Epoxy Networks

Saraf

Stubbs

et al. 2020

Macro Materials & Eng

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Multifunctional organophosphorus additives present opportunities to engineer epoxy networks with both enhanced mechanical properties and ultralow flammability. This paper describes a systematic investigation of the effect of dimethyl methylphosphonate (DMMP) on the mechanical and heat release properties of both conventional and inherently low flammability epoxy resins. The findings demonstrate that integration of DMMP into epoxy networks produces materials with outstanding flame retardance and increased stiffness. Thermogravimetric analysis of DMMP‐containing networks show that DMMP promotes considerable char formation, with char residue reaching very high levels, up to 55%, for DMMP‐containing deoxybenzoin networks. Microscale combustion calorimetry of all the DMMP‐containing networks exhibit 50% lower heat release capacity and total heat release rate values relative to formulations without DMMP. Moreover, vertical burn tests demonstrate that DMMP‐containing formulations burn slowly and self‐extinguish. Morphological analysis of the charred DMMP‐containing formulations shows a porous structure and mechanical characterization reveals 50% higher elastic modulus, and comparable yield stress, for networks containing DMMP relative to those without DMMP. Overall, this organophosphorus additive represents an opportunity to combine materials chemistry with mechanical enhancement mechanisms to achieve low heat release properties without the need for halogenated flame‐retardant additives.

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Combining Mechanical Fortification and Ultralow Flammability in Epoxy Networks

Saraf

Stubbs

et al. 2020

Macro Materials & Eng

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Joint‐aggregation intumescent flame‐retardant effect of ammonium polyphosphate and charring agent in polypropylene

Tang

Qian

Chen

et al. 2020

Polymers for Advanced Techs

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In order to explore the structure mode of intumescent flame retardants (IFRs) with higher efficiency, IFR particles with joint‐aggregation structure (@IFR) were obtained through the treatment of ammonium polyphosphate (APP) and a charring agent (PT‐Cluster) in their aqueous solution. Then, the joint‐aggregation IFR effect was researched using its application in polypropylene. In case of 20 wt% IFR loading, the limiting oxygen index (LOI) value of @IFR/PP was 1.1% higher than that of 15APP/5PT‐Cluster/PP mixture, and a 1.6 mm‐thick @IFR/PP composite passed the UL 94 V‐2 rating test, while 15APP/5PT‐Cluster/PP demonstrated no flame‐retardant rating in UL 94 vertical burning tests. In a cone calorimeter test, @IFR also had a better inhibition effect on heat release. The average heat release rate (av‐HRR) value during 0 to 120 seconds of @IFR/PP was only 41 kW m−2, which was 33.9% lower than that of the 15APP/5PT‐Cluster/PP. Furthermore, the peak heat release rate (pk‐HRR) of @IFR/PP was 20.5% lower than that of 15APP/5PT‐Cluster/PP, and the time to pk‐HRR of @IFR/PP was 710 seconds, while that of 15APP/5PT‐Cluster/PP was 580 seconds. The better inhibition effect on HRR and the delay of time to pk‐HRR were caused by the joint‐aggregated structure of @IFR, which can rapidly react to form stable and efficient char layers. This kind of join‐aggregation IFR effect has great significance in suppressing the spread of fire in reality. In addition, @IFR also increased the mechanical properties of PP composites slightly compared with the APP/PT‐Cluster mixture.

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The synergism effect of montmorillonite on the intumescent flame retardant thermoplastic polyurethane composites prepared by selective laser sintering

Hu³

et al. 2022

Polymer Composites

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Selective Laser Sintering (SLS) is a powder‐based 3D printing technology. It offers a new means of fabricating complex modules with special properties, such as mechanical, flame retardant, electrical and thermal properties. In this paper, the effect of an intumescent flame retardant (IFR) and montmorillonite (MMT) on the fire resistance of thermoplastic polyurethane (TPU) was investigated. TPU composites powders were prepared by mixing with a two‐step method and can be effectively applied to SLS. Morphology characters exhibited that the fillers disperse well in the TPU powder. The structure analysis and hydrophilia analysis of sodium montmorillonite (Na‐MMT) and organically modified montmorillonite (OMMT) demonstrates the different compatibility in TPU, which reflects diverse flame retardant behavior. With 22% IFR and 3% OMMT fillers, the LOI of TPU composites increased from 17.2% to 28% and subsequently a UL‐94 V‐0 ranking was obtained. In the CCT results, the formula of 22% IFR and 3% OMMT showed the lowest heat release and smoke production. The study also explored the effects of flame retardant fillers on the thermal stability of TPU composites and melting and crystallization behaviors in SLS processing. In addition, the char residues after heating were analyzed via scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, Fourier transform infrared spectroscopy and laser Raman spectroscopy. The results demonstrate that the composites have favorable flame retardant properties, thermal stability, char forming performance, and SLS process properties. The TPU composites prepared via SLS in this study demonstrated extensive potential in fire protection materials.

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Synthesis of charring agent and its derivatives of dipentaerythritol polycyclicphosphonates flame retardants

Cited by 4 publications

References 33 publications

Combining Mechanical Fortification and Ultralow Flammability in Epoxy Networks

Combining Mechanical Fortification and Ultralow Flammability in Epoxy Networks

Joint‐aggregation intumescent flame‐retardant effect of ammonium polyphosphate and charring agent in polypropylene

The synergism effect of montmorillonite on the intumescent flame retardant thermoplastic polyurethane composites prepared by selective laser sintering

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