ICGM, Université de Montpellier, CNRS, ENSCM, 34000 Montpellier, France.
Polymers Composites and Hybrids (PCH), IMT Mines Ales, 30100 Ales, France.
Molecules. 2023 Jan 6;28(2):611. doi: 10.3390/molecules28020611.
This article focuses on the synthesis of polyhydroxyurethane (PHU) materials containing novel phosphorus flame retardants (FR). Four different phosphorus compounds were grafted onto cyclic carbonate: 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), diethyl phosphite (DEP), diphenyl phosphite (DPP) and dibenzo[d,f][1,3,2]dioxaphosphepine 6-oxide (BPPO). Thus, three novel phosphorus reactive cyclic carbonates which have never been reported so far were synthetized. Phosphorus FR containing PHU materials were characterized by FTIR to evidence the total conversion of the cyclic carbonate. Moreover, the gel contents up to 80% confirmed the formation of the polymer network. Then, the thermal stability and the flame-retardant properties were investigated by thermogravimetric analyses, cone calorimeter and pyrolysis combustion flow calorimeter. The mode of action of phosphorus compounds, depending on the oxidation state, was especially highlighted. Phosphonate (+III) provided better action in a condensed phase than phosphinate thanks to a more efficient char formation. Among phosphonates, differences were observed in terms of char-formation rate and expansion. DEP provided the best flame-retardant properties, with a reduction of 76% of pHRR with 2 wt% of phosphorus in cone calorimeter analysis. Therefore, this article highlighted the different modes of action of phosphorus flame retardants, depending on the oxidation state of phosphorus, in PHU materials.
本文专注于含有新型磷系阻燃剂 (FR) 的聚碳酸酯型多羟基聚氨酯 (PHU) 材料的合成。四种不同的磷化合物被接枝到环状碳酸酯上:9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物 (DOPO)、亚磷酸二乙酯 (DEP)、亚磷酸二苯酯 (DPP) 和二苯并[d,f][1,3,2]二氧杂磷杂环戊二烯 6-氧化物 (BPPO)。因此,三种新型磷系反应性环状碳酸酯被合成,迄今为止尚未有报道。含磷阻燃剂的 PHU 材料通过傅里叶变换红外光谱 (FTIR) 进行了表征,以证明环状碳酸酯的完全转化。此外,凝胶含量高达 80%,证实了聚合物网络的形成。然后,通过热重分析、锥形量热仪和热解燃烧流动量热仪研究了热稳定性和阻燃性能。磷化合物的作用模式,取决于氧化态,特别是被强调。由于更有效的炭形成,亚磷酸酯 (+III) 在凝聚相中提供了比膦酸酯更好的作用。在亚磷酸酯中,观察到炭形成速率和膨胀方面的差异。在锥形量热仪分析中,DEP 提供了最好的阻燃性能,添加 2wt%磷时,总热释放量 (pHRR) 降低了 76%。因此,本文强调了磷系阻燃剂在 PHU 材料中的不同作用模式,取决于磷的氧化态。